# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_LNiClPy2
_database_code_depnum_ccdc_archive 'CCDC 1953729'
loop_
_audit_author_name
_audit_author_address
'Shao-Liang Zheng'
;Harvard Univerisity
United States of America
;
_audit_update_record
;
2019-09-16 deposited with the CCDC. 2019-12-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C45 H44 Cl F5 N4 Ni'
_chemical_formula_weight 830.00
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 19.2423(8)
_cell_length_b 10.9261(5)
_cell_length_c 21.5899(10)
_cell_angle_alpha 90
_cell_angle_beta 106.046(2)
_cell_angle_gamma 90
_cell_volume 4362.3(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9954
_cell_measurement_theta_min 4.27
_cell_measurement_theta_max 66.76
_exptl_crystal_description plate
_exptl_crystal_colour pink
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.264
_exptl_crystal_F_000 1728
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.110
_exptl_absorpt_coefficient_mu 1.674
_shelx_estimated_absorpt_T_min 0.670
_shelx_estimated_absorpt_T_max 0.837
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5601
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details SADBAS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source 'I/mS microfocus tube'
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 57252
_diffrn_reflns_av_unetI/netI 0.0493
_diffrn_reflns_av_R_equivalents 0.0843
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 2.389
_diffrn_reflns_theta_max 66.813
_diffrn_reflns_theta_full 66.813
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total 7681
_reflns_number_gt 6417
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_cell_refinement 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_reduction 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. All non H-atoms were located in difference-Fourier maps, and then refined anisotropically. The disorder solvent could not be located in the Fourier map and have been squeezed out by using solvent mask from Olex2.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+1.3876P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 7681
_refine_ls_number_parameters 505
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0526
_refine_ls_R_factor_gt 0.0443
_refine_ls_wR_factor_ref 0.1273
_refine_ls_wR_factor_gt 0.1209
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.20743(2) 0.39078(3) 0.68783(2) 0.02164(12) Uani 1 1 d . . . . .
Cl1 Cl 0.08222(3) 0.38187(4) 0.66082(2) 0.02546(13) Uani 1 1 d . . . . .
N2 N 0.28339(9) 0.28008(15) 0.74510(8) 0.0203(3) Uani 1 1 d . . . . .
N1 N 0.27662(9) 0.51083(15) 0.66333(8) 0.0217(4) Uani 1 1 d . . . . .
F5 F 0.46140(9) 0.27295(18) 0.64808(9) 0.0636(5) Uani 1 1 d . . . . .
F3 F 0.68945(8) 0.38434(17) 0.78029(10) 0.0725(6) Uani 1 1 d . . . . .
N4 N 0.20795(9) 0.27786(15) 0.60347(8) 0.0244(4) Uani 1 1 d . . . . .
N3 N 0.20979(9) 0.50393(15) 0.77232(8) 0.0240(4) Uani 1 1 d . . . . .
F1 F 0.48022(9) 0.51918(19) 0.82917(10) 0.0767(6) Uani 1 1 d . . . . .
F4 F 0.60696(11) 0.2662(2) 0.67505(11) 0.0892(7) Uani 1 1 d . . . . .
F2 F 0.62603(10) 0.5102(2) 0.85657(13) 0.0958(8) Uani 1 1 d . . . . .
C6 C 0.35704(11) 0.30079(18) 0.75204(10) 0.0228(4) Uani 1 1 d . . . . .
C21 C 0.19355(11) 0.66714(17) 0.59328(9) 0.0206(4) Uani 1 1 d . . . . .
C5 C 0.26644(11) 0.61257(17) 0.62668(10) 0.0228(4) Uani 1 1 d . . . . .
C2 C 0.35138(11) 0.49162(18) 0.68456(10) 0.0235(4) Uani 1 1 d . . . . .
C25 C 0.12944(12) 0.83652(19) 0.51867(10) 0.0267(5) Uani 1 1 d . . . . .
H25 H 0.1371 0.9095 0.4933 0.032 Uiso 1 1 calc R U . . .
C1 C 0.38578(11) 0.39649(18) 0.72398(10) 0.0245(4) Uani 1 1 d . . . . .
C9 C 0.27939(11) 0.18128(18) 0.78125(10) 0.0215(4) Uani 1 1 d . . . . .
C29 C 0.07266(11) 0.63013(18) 0.51174(10) 0.0238(4) Uani 1 1 d . . . . .
H29 H 0.0426 0.5681 0.4821 0.029 Uiso 1 1 calc R U . . .
C7 C 0.39834(11) 0.21072(19) 0.79409(11) 0.0276(5) Uani 1 1 d . . . . .
H7 H 0.4495 0.2034 0.8070 0.033 Uiso 1 1 calc R U . . .
C24 C 0.20299(11) 0.78080(19) 0.55391(10) 0.0262(5) Uani 1 1 d . . . . .
H24A H 0.2325 0.8427 0.5832 0.031 Uiso 1 1 calc R U . . .
H24B H 0.2290 0.7573 0.5221 0.031 Uiso 1 1 calc R U . . .
C23 C 0.14631(11) 0.57421(18) 0.54595(10) 0.0230(4) Uani 1 1 d . . . . .
H23A H 0.1714 0.5495 0.5136 0.028 Uiso 1 1 calc R U . . .
H23B H 0.1392 0.5001 0.5698 0.028 Uiso 1 1 calc R U . . .
C30 C 0.08342(12) 0.74174(19) 0.47297(10) 0.0265(5) Uani 1 1 d . . . . .
H30A H 0.0359 0.7776 0.4504 0.032 Uiso 1 1 calc R U . . .
H30B H 0.1079 0.7172 0.4402 0.032 Uiso 1 1 calc R U . . .
C31 C 0.21072(11) 0.12642(18) 0.79004(10) 0.0231(4) Uani 1 1 d . . . . .
C34 C 0.17044(11) 0.22218(19) 0.81981(11) 0.0262(5) Uani 1 1 d . . . . .
H34A H 0.2025 0.2510 0.8614 0.031 Uiso 1 1 calc R U . . .
H34B H 0.1575 0.2935 0.7906 0.031 Uiso 1 1 calc R U . . .
C27 C 0.07952(11) 0.76450(18) 0.60755(10) 0.0246(4) Uani 1 1 d . . . . .
H27 H 0.0540 0.7900 0.6400 0.030 Uiso 1 1 calc R U . . .
C26 C 0.09042(12) 0.87609(18) 0.56841(11) 0.0277(5) Uani 1 1 d . . . . .
H26A H 0.1195 0.9386 0.5975 0.033 Uiso 1 1 calc R U . . .
H26B H 0.0430 0.9125 0.5462 0.033 Uiso 1 1 calc R U . . .
C8 C 0.35017(11) 0.1366(2) 0.81235(11) 0.0276(5) Uani 1 1 d . . . . .
H8 H 0.3617 0.0682 0.8405 0.033 Uiso 1 1 calc R U . . .
C22 C 0.15310(11) 0.70813(18) 0.64235(10) 0.0232(4) Uani 1 1 d . . . . .
H22A H 0.1457 0.6368 0.6681 0.028 Uiso 1 1 calc R U . . .
H22B H 0.1826 0.7691 0.6722 0.028 Uiso 1 1 calc R U . . .
C4 C 0.33410(12) 0.6604(2) 0.62355(11) 0.0294(5) Uani 1 1 d . . . . .
H4 H 0.3412 0.7316 0.6008 0.035 Uiso 1 1 calc R U . . .
C11 C 0.46673(12) 0.39512(19) 0.73845(12) 0.0287(5) Uani 1 1 d . . . . .
C3 C 0.38678(12) 0.5858(2) 0.65908(11) 0.0298(5) Uani 1 1 d . . . . .
H3 H 0.4374 0.5948 0.6656 0.036 Uiso 1 1 calc R U . . .
C28 C 0.03427(11) 0.66816(18) 0.56238(10) 0.0247(4) Uani 1 1 d . . . . .
H28A H -0.0140 0.7022 0.5407 0.030 Uiso 1 1 calc R U . . .
H28B H 0.0275 0.5957 0.5876 0.030 Uiso 1 1 calc R U . . .
C35 C 0.10153(12) 0.1660(2) 0.83068(12) 0.0319(5) Uani 1 1 d . . . . .
H35 H 0.0760 0.2295 0.8496 0.038 Uiso 1 1 calc R U . . .
C32 C 0.22882(12) 0.0161(2) 0.83689(11) 0.0298(5) Uani 1 1 d . . . . .
H32A H 0.2544 -0.0473 0.8189 0.036 Uiso 1 1 calc R U . . .
H32B H 0.2612 0.0431 0.8787 0.036 Uiso 1 1 calc R U . . .
C41 C 0.15113(12) 0.5361(2) 0.78985(11) 0.0294(5) Uani 1 1 d . . . . .
H41 H 0.1051 0.5122 0.7632 0.035 Uiso 1 1 calc R U . . .
C37 C 0.15980(13) -0.0383(2) 0.84745(12) 0.0351(5) Uani 1 1 d . . . . .
H37 H 0.1729 -0.1093 0.8777 0.042 Uiso 1 1 calc R U . . .
C45 C 0.27402(13) 0.5393(2) 0.81022(11) 0.0333(5) Uani 1 1 d . . . . .
H45 H 0.3164 0.5184 0.7981 0.040 Uiso 1 1 calc R U . . .
C46 C 0.14860(12) 0.23524(19) 0.56099(11) 0.0309(5) Uani 1 1 d . . . . .
H46 H 0.1029 0.2516 0.5681 0.037 Uiso 1 1 calc R U . . .
C42 C 0.15414(14) 0.6027(2) 0.84510(12) 0.0363(6) Uani 1 1 d . . . . .
H42 H 0.1110 0.6244 0.8558 0.044 Uiso 1 1 calc R U . . .
C33 C 0.16004(12) 0.0808(2) 0.72597(11) 0.0282(5) Uani 1 1 d . . . . .
H33A H 0.1851 0.0178 0.7071 0.034 Uiso 1 1 calc R U . . .
H33B H 0.1473 0.1497 0.6952 0.034 Uiso 1 1 calc R U . . .
C36 C 0.12109(14) 0.0583(2) 0.87704(12) 0.0365(5) Uani 1 1 d . . . . .
H36A H 0.0768 0.0231 0.8846 0.044 Uiso 1 1 calc R U . . .
H36B H 0.1531 0.0861 0.9189 0.044 Uiso 1 1 calc R U . . .
C39 C 0.09063(13) 0.0260(2) 0.73694(12) 0.0345(5) Uani 1 1 d . . . . .
H39 H 0.0580 -0.0022 0.6948 0.041 Uiso 1 1 calc R U . . .
C43 C 0.22023(14) 0.6366(2) 0.88409(11) 0.0366(6) Uani 1 1 d . . . . .
H43 H 0.2238 0.6811 0.9227 0.044 Uiso 1 1 calc R U . . .
C44 C 0.28135(14) 0.6054(2) 0.86659(12) 0.0381(6) Uani 1 1 d . . . . .
H44 H 0.3278 0.6287 0.8926 0.046 Uiso 1 1 calc R U . . .
C48 C 0.21591(13) 0.1444(2) 0.49552(11) 0.0332(5) Uani 1 1 d . . . . .
H48 H 0.2183 0.0991 0.4586 0.040 Uiso 1 1 calc R U . . .
C16 C 0.50131(13) 0.3322(2) 0.69998(13) 0.0391(6) Uani 1 1 d . . . . .
C38 C 0.11010(13) -0.0827(2) 0.78330(13) 0.0377(6) Uani 1 1 d . . . . .
H38A H 0.0656 -0.1186 0.7902 0.045 Uiso 1 1 calc R U . . .
H38B H 0.1348 -0.1465 0.7647 0.045 Uiso 1 1 calc R U . . .
C40 C 0.05176(12) 0.1238(2) 0.76629(13) 0.0353(6) Uani 1 1 d . . . . .
H40A H 0.0387 0.1944 0.7366 0.042 Uiso 1 1 calc R U . . .
H40B H 0.0067 0.0894 0.7728 0.042 Uiso 1 1 calc R U . . .
C47 C 0.15052(13) 0.1687(2) 0.50734(12) 0.0369(6) Uani 1 1 d . . . . .
H47 H 0.1069 0.1396 0.4786 0.044 Uiso 1 1 calc R U . . .
C12 C 0.51084(13) 0.4556(2) 0.79108(14) 0.0424(6) Uani 1 1 d . . . . .
C14 C 0.61733(13) 0.3879(3) 0.76658(16) 0.0499(8) Uani 1 1 d . . . . .
C50 C 0.27057(14) 0.2533(3) 0.59179(13) 0.0419(6) Uani 1 1 d . . . . .
H50 H 0.3135 0.2824 0.6215 0.050 Uiso 1 1 calc R U . . .
C49 C 0.27695(15) 0.1872(3) 0.53838(13) 0.0443(6) Uani 1 1 d . . . . .
H49 H 0.3231 0.1722 0.5320 0.053 Uiso 1 1 calc R U . . .
C13 C 0.58501(14) 0.4522(3) 0.80538(16) 0.0514(7) Uani 1 1 d . . . . .
C15 C 0.57542(14) 0.3277(3) 0.71378(16) 0.0497(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0193(2) 0.0228(2) 0.0249(2) -0.00071(13) 0.00970(15) -0.00059(13)
Cl1 0.0208(3) 0.0288(3) 0.0287(3) 0.00267(18) 0.0101(2) 0.00259(18)
N2 0.0189(8) 0.0213(9) 0.0235(9) -0.0030(6) 0.0106(7) 0.0001(6)
N1 0.0220(9) 0.0208(9) 0.0243(9) -0.0016(6) 0.0101(7) -0.0009(6)
F5 0.0461(10) 0.0902(13) 0.0612(11) -0.0256(9) 0.0258(9) 0.0109(9)
F3 0.0166(7) 0.0885(14) 0.1127(16) 0.0610(11) 0.0182(9) 0.0085(7)
N4 0.0253(9) 0.0229(9) 0.0275(9) 0.0004(7) 0.0115(7) -0.0006(7)
N3 0.0285(10) 0.0212(9) 0.0254(9) 0.0003(7) 0.0125(8) 0.0008(7)
F1 0.0388(9) 0.0987(15) 0.0846(14) -0.0595(12) 0.0037(9) -0.0044(9)
F4 0.0547(12) 0.1251(18) 0.1073(17) 0.0088(13) 0.0551(12) 0.0381(12)
F2 0.0332(10) 0.1153(18) 0.1192(19) -0.0309(14) -0.0120(11) -0.0212(10)
C6 0.0199(10) 0.0229(10) 0.0285(11) -0.0028(8) 0.0116(8) 0.0003(8)
C21 0.0232(10) 0.0188(10) 0.0223(10) -0.0003(7) 0.0108(8) -0.0026(8)
C5 0.0253(11) 0.0217(11) 0.0243(11) -0.0027(7) 0.0119(9) -0.0014(8)
C2 0.0193(10) 0.0246(11) 0.0289(11) -0.0031(8) 0.0105(9) -0.0034(8)
C25 0.0330(12) 0.0213(11) 0.0278(11) 0.0044(8) 0.0120(9) -0.0010(9)
C1 0.0238(11) 0.0234(11) 0.0292(11) -0.0045(8) 0.0120(9) -0.0012(8)
C9 0.0231(10) 0.0209(10) 0.0237(10) -0.0046(7) 0.0117(8) 0.0010(8)
C29 0.0273(11) 0.0217(11) 0.0228(11) -0.0021(8) 0.0075(9) -0.0017(8)
C7 0.0203(11) 0.0283(12) 0.0351(12) 0.0004(9) 0.0094(9) 0.0038(8)
C24 0.0289(11) 0.0244(11) 0.0280(11) 0.0003(8) 0.0123(9) -0.0040(8)
C23 0.0264(11) 0.0211(10) 0.0242(11) -0.0030(8) 0.0113(9) -0.0016(8)
C30 0.0278(11) 0.0281(12) 0.0244(11) 0.0014(8) 0.0083(9) -0.0011(8)
C31 0.0258(11) 0.0201(10) 0.0276(11) 0.0007(8) 0.0143(9) 0.0004(8)
C34 0.0284(11) 0.0227(11) 0.0315(12) -0.0008(8) 0.0147(9) 0.0019(8)
C27 0.0280(11) 0.0240(11) 0.0247(11) -0.0003(8) 0.0120(9) 0.0022(8)
C26 0.0294(12) 0.0231(11) 0.0304(12) -0.0005(8) 0.0081(9) 0.0004(8)
C8 0.0264(11) 0.0255(11) 0.0323(12) 0.0036(8) 0.0102(9) 0.0022(8)
C22 0.0260(11) 0.0223(11) 0.0236(10) -0.0022(8) 0.0106(9) -0.0009(8)
C4 0.0264(11) 0.0261(12) 0.0387(13) 0.0036(9) 0.0138(10) -0.0041(9)
C11 0.0205(11) 0.0262(12) 0.0414(13) 0.0058(9) 0.0118(10) 0.0004(8)
C3 0.0205(11) 0.0323(12) 0.0389(13) 0.0011(9) 0.0122(9) -0.0029(9)
C28 0.0223(11) 0.0242(11) 0.0297(11) 0.0023(8) 0.0106(9) -0.0001(8)
C35 0.0346(12) 0.0279(12) 0.0428(14) 0.0038(9) 0.0269(11) 0.0036(9)
C32 0.0314(12) 0.0272(12) 0.0362(13) 0.0058(9) 0.0183(10) 0.0072(9)
C41 0.0322(12) 0.0278(12) 0.0309(12) 0.0012(8) 0.0129(10) 0.0081(9)
C37 0.0418(14) 0.0267(12) 0.0453(14) 0.0093(9) 0.0264(11) 0.0049(10)
C45 0.0318(12) 0.0375(13) 0.0342(13) -0.0078(9) 0.0151(10) -0.0047(10)
C46 0.0290(12) 0.0242(11) 0.0372(13) -0.0052(9) 0.0051(10) 0.0023(8)
C42 0.0460(15) 0.0353(13) 0.0326(13) -0.0015(9) 0.0192(11) 0.0116(10)
C33 0.0290(12) 0.0278(12) 0.0309(12) -0.0028(9) 0.0133(9) -0.0034(9)
C36 0.0401(14) 0.0343(13) 0.0445(14) 0.0087(10) 0.0276(12) 0.0055(10)
C39 0.0329(13) 0.0308(12) 0.0426(14) -0.0032(10) 0.0148(11) -0.0089(9)
C43 0.0560(16) 0.0304(12) 0.0289(12) -0.0039(9) 0.0208(12) 0.0033(11)
C44 0.0419(14) 0.0425(15) 0.0324(13) -0.0098(10) 0.0144(11) -0.0112(10)
C48 0.0512(15) 0.0249(11) 0.0252(12) -0.0014(8) 0.0134(11) 0.0026(10)
C16 0.0299(13) 0.0438(15) 0.0493(16) 0.0061(11) 0.0206(11) 0.0052(10)
C38 0.0371(13) 0.0262(12) 0.0583(16) -0.0013(10) 0.0276(12) -0.0044(10)
C40 0.0249(12) 0.0328(13) 0.0538(16) 0.0088(10) 0.0201(11) -0.0017(9)
C47 0.0383(14) 0.0286(13) 0.0369(14) -0.0092(9) -0.0011(11) 0.0044(10)
C12 0.0258(12) 0.0404(15) 0.0590(17) -0.0071(12) 0.0084(12) -0.0051(10)
C14 0.0206(12) 0.0498(17) 0.082(2) 0.0379(15) 0.0182(14) 0.0060(11)
C50 0.0300(13) 0.0594(17) 0.0388(14) -0.0202(11) 0.0138(11) -0.0054(11)
C49 0.0396(14) 0.0592(17) 0.0406(15) -0.0182(12) 0.0221(12) -0.0048(12)
C13 0.0258(13) 0.0508(17) 0.070(2) 0.0070(14) 0.0004(13) -0.0110(11)
C15 0.0326(14) 0.0583(18) 0.070(2) 0.0229(14) 0.0332(14) 0.0164(12)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.0320(17) . ?
Ni1 N1 2.0401(16) . ?
Ni1 N3 2.1936(17) . ?
Ni1 N4 2.2022(17) . ?
Ni1 Cl1 2.3190(6) . ?
N2 C9 1.347(3) . ?
N2 C6 1.402(3) . ?
N1 C5 1.347(3) . ?
N1 C2 1.400(3) . ?
F5 C16 1.337(3) . ?
F3 C14 1.337(3) . ?
N4 C50 1.325(3) . ?
N4 C46 1.335(3) . ?
N3 C41 1.333(3) . ?
N3 C45 1.337(3) . ?
F1 C12 1.332(3) . ?
F4 C15 1.342(3) . ?
F2 C13 1.328(3) . ?
C6 C1 1.397(3) . ?
C6 C7 1.423(3) . ?
C21 C5 1.511(3) . ?
C21 C24 1.544(3) . ?
C21 C22 1.544(3) . ?
C21 C23 1.545(3) . ?
C5 C4 1.422(3) . ?
C2 C1 1.390(3) . ?
C2 C3 1.426(3) . ?
C25 C30 1.532(3) . ?
C25 C26 1.533(3) . ?
C25 C24 1.535(3) . ?
C25 H25 1.0000 . ?
C1 C11 1.502(3) . ?
C9 C8 1.428(3) . ?
C9 C31 1.510(3) . ?
C29 C30 1.525(3) . ?
C29 C23 1.533(3) . ?
C29 C28 1.536(3) . ?
C29 H29 1.0000 . ?
C7 C8 1.368(3) . ?
C7 H7 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C33 1.539(3) . ?
C31 C34 1.544(3) . ?
C31 C32 1.550(3) . ?
C34 C35 1.537(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C27 C26 1.531(3) . ?
C27 C28 1.532(3) . ?
C27 C22 1.536(3) . ?
C27 H27 1.0000 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C8 H8 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C4 C3 1.361(3) . ?
C4 H4 0.9500 . ?
C11 C16 1.383(3) . ?
C11 C12 1.384(3) . ?
C3 H3 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C35 C36 1.523(3) . ?
C35 C40 1.525(4) . ?
C35 H35 1.0000 . ?
C32 C37 1.528(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C41 C42 1.385(3) . ?
C41 H41 0.9500 . ?
C37 C38 1.528(4) . ?
C37 C36 1.530(3) . ?
C37 H37 1.0000 . ?
C45 C44 1.388(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.377(3) . ?
C46 H46 0.9500 . ?
C42 C43 1.368(4) . ?
C42 H42 0.9500 . ?
C33 C39 1.540(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C39 C38 1.531(3) . ?
C39 C40 1.538(3) . ?
C39 H39 1.0000 . ?
C43 C44 1.374(3) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C48 C49 1.362(4) . ?
C48 C47 1.377(3) . ?
C48 H48 0.9500 . ?
C16 C15 1.375(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C47 H47 0.9500 . ?
C12 C13 1.375(4) . ?
C14 C13 1.367(4) . ?
C14 C15 1.369(5) . ?
C50 C49 1.395(3) . ?
C50 H50 0.9500 . ?
C49 H49 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N1 97.43(7) . . ?
N2 Ni1 N3 89.05(6) . . ?
N1 Ni1 N3 89.33(6) . . ?
N2 Ni1 N4 90.16(6) . . ?
N1 Ni1 N4 89.62(6) . . ?
N3 Ni1 N4 178.59(7) . . ?
N2 Ni1 Cl1 130.59(5) . . ?
N1 Ni1 Cl1 131.98(5) . . ?
N3 Ni1 Cl1 90.81(5) . . ?
N4 Ni1 Cl1 90.60(5) . . ?
C9 N2 C6 106.59(16) . . ?
C9 N2 Ni1 133.09(13) . . ?
C6 N2 Ni1 120.32(13) . . ?
C5 N1 C2 106.59(16) . . ?
C5 N1 Ni1 133.12(14) . . ?
C2 N1 Ni1 120.26(13) . . ?
C50 N4 C46 116.66(19) . . ?
C50 N4 Ni1 118.89(15) . . ?
C46 N4 Ni1 124.39(15) . . ?
C41 N3 C45 117.52(19) . . ?
C41 N3 Ni1 124.06(15) . . ?
C45 N3 Ni1 118.37(14) . . ?
C1 C6 N2 125.76(19) . . ?
C1 C6 C7 125.17(19) . . ?
N2 C6 C7 109.05(17) . . ?
C5 C21 C24 110.20(16) . . ?
C5 C21 C22 111.37(16) . . ?
C24 C21 C22 107.62(16) . . ?
C5 C21 C23 110.79(16) . . ?
C24 C21 C23 107.56(16) . . ?
C22 C21 C23 109.17(16) . . ?
N1 C5 C4 110.19(19) . . ?
N1 C5 C21 124.82(18) . . ?
C4 C5 C21 124.98(18) . . ?
C1 C2 N1 125.81(18) . . ?
C1 C2 C3 125.36(19) . . ?
N1 C2 C3 108.83(18) . . ?
C30 C25 C26 109.52(17) . . ?
C30 C25 C24 109.92(17) . . ?
C26 C25 C24 109.13(17) . . ?
C30 C25 H25 109.4 . . ?
C26 C25 H25 109.4 . . ?
C24 C25 H25 109.4 . . ?
C2 C1 C6 130.29(19) . . ?
C2 C1 C11 115.21(18) . . ?
C6 C1 C11 114.49(18) . . ?
N2 C9 C8 110.28(18) . . ?
N2 C9 C31 125.68(18) . . ?
C8 C9 C31 124.02(19) . . ?
C30 C29 C23 109.61(17) . . ?
C30 C29 C28 109.83(16) . . ?
C23 C29 C28 109.11(16) . . ?
C30 C29 H29 109.4 . . ?
C23 C29 H29 109.4 . . ?
C28 C29 H29 109.4 . . ?
C8 C7 C6 106.83(19) . . ?
C8 C7 H7 126.6 . . ?
C6 C7 H7 126.6 . . ?
C25 C24 C21 111.05(16) . . ?
C25 C24 H24A 109.4 . . ?
C21 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C21 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C29 C23 C21 110.69(16) . . ?
C29 C23 H23A 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C29 C23 H23B 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C29 C30 C25 109.20(17) . . ?
C29 C30 H30A 109.8 . . ?
C25 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
C25 C30 H30B 109.8 . . ?
H30A C30 H30B 108.3 . . ?
C9 C31 C33 112.01(17) . . ?
C9 C31 C34 109.92(16) . . ?
C33 C31 C34 109.12(17) . . ?
C9 C31 C32 110.13(17) . . ?
C33 C31 C32 107.86(17) . . ?
C34 C31 C32 107.67(17) . . ?
C35 C34 C31 110.27(17) . . ?
C35 C34 H34A 109.6 . . ?
C31 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C31 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C26 C27 C28 109.65(17) . . ?
C26 C27 C22 109.94(17) . . ?
C28 C27 C22 108.70(16) . . ?
C26 C27 H27 109.5 . . ?
C28 C27 H27 109.5 . . ?
C22 C27 H27 109.5 . . ?
C27 C26 C25 109.30(16) . . ?
C27 C26 H26A 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
C7 C8 C9 107.25(19) . . ?
C7 C8 H8 126.4 . . ?
C9 C8 H8 126.4 . . ?
C27 C22 C21 110.60(16) . . ?
C27 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C27 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C3 C4 C5 107.58(19) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
C16 C11 C12 116.3(2) . . ?
C16 C11 C1 121.6(2) . . ?
C12 C11 C1 122.1(2) . . ?
C4 C3 C2 106.81(19) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
C27 C28 C29 109.77(16) . . ?
C27 C28 H28A 109.7 . . ?
C29 C28 H28A 109.7 . . ?
C27 C28 H28B 109.7 . . ?
C29 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C36 C35 C40 110.2(2) . . ?
C36 C35 C34 110.00(19) . . ?
C40 C35 C34 109.42(18) . . ?
C36 C35 H35 109.1 . . ?
C40 C35 H35 109.1 . . ?
C34 C35 H35 109.1 . . ?
C37 C32 C31 110.60(18) . . ?
C37 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C37 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
N3 C41 C42 123.1(2) . . ?
N3 C41 H41 118.5 . . ?
C42 C41 H41 118.5 . . ?
C38 C37 C32 109.88(19) . . ?
C38 C37 C36 110.0(2) . . ?
C32 C37 C36 109.73(19) . . ?
C38 C37 H37 109.1 . . ?
C32 C37 H37 109.1 . . ?
C36 C37 H37 109.1 . . ?
N3 C45 C44 122.7(2) . . ?
N3 C45 H45 118.7 . . ?
C44 C45 H45 118.7 . . ?
N4 C46 C47 123.0(2) . . ?
N4 C46 H46 118.5 . . ?
C47 C46 H46 118.5 . . ?
C43 C42 C41 118.9(2) . . ?
C43 C42 H42 120.6 . . ?
C41 C42 H42 120.6 . . ?
C31 C33 C39 110.41(18) . . ?
C31 C33 H33A 109.6 . . ?
C39 C33 H33A 109.6 . . ?
C31 C33 H33B 109.6 . . ?
C39 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C35 C36 C37 108.59(19) . . ?
C35 C36 H36A 110.0 . . ?
C37 C36 H36A 110.0 . . ?
C35 C36 H36B 110.0 . . ?
C37 C36 H36B 110.0 . . ?
H36A C36 H36B 108.4 . . ?
C38 C39 C40 109.2(2) . . ?
C38 C39 C33 109.6(2) . . ?
C40 C39 C33 109.55(18) . . ?
C38 C39 H39 109.5 . . ?
C40 C39 H39 109.5 . . ?
C33 C39 H39 109.5 . . ?
C42 C43 C44 119.0(2) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 H43 120.5 . . ?
C43 C44 C45 118.9(2) . . ?
C43 C44 H44 120.6 . . ?
C45 C44 H44 120.6 . . ?
C49 C48 C47 117.9(2) . . ?
C49 C48 H48 121.0 . . ?
C47 C48 H48 121.0 . . ?
F5 C16 C15 119.0(2) . . ?
F5 C16 C11 118.9(2) . . ?
C15 C16 C11 122.0(3) . . ?
C37 C38 C39 108.97(19) . . ?
C37 C38 H38A 109.9 . . ?
C39 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
C39 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
C35 C40 C39 109.34(19) . . ?
C35 C40 H40A 109.8 . . ?
C39 C40 H40A 109.8 . . ?
C35 C40 H40B 109.8 . . ?
C39 C40 H40B 109.8 . . ?
H40A C40 H40B 108.3 . . ?
C46 C47 C48 119.8(2) . . ?
C46 C47 H47 120.1 . . ?
C48 C47 H47 120.1 . . ?
F1 C12 C13 119.0(2) . . ?
F1 C12 C11 118.7(2) . . ?
C13 C12 C11 122.3(3) . . ?
F3 C14 C13 120.0(3) . . ?
F3 C14 C15 120.5(3) . . ?
C13 C14 C15 119.6(2) . . ?
N4 C50 C49 123.7(2) . . ?
N4 C50 H50 118.2 . . ?
C49 C50 H50 118.2 . . ?
C48 C49 C50 118.9(2) . . ?
C48 C49 H49 120.5 . . ?
C50 C49 H49 120.5 . . ?
F2 C13 C14 119.2(3) . . ?
F2 C13 C12 121.0(3) . . ?
C14 C13 C12 119.8(3) . . ?
F4 C15 C14 119.7(2) . . ?
F4 C15 C16 120.2(3) . . ?
C14 C15 C16 120.0(3) . . ?
_refine_diff_density_max 0.508
_refine_diff_density_min -0.657
_refine_diff_density_rms 0.058
_shelx_res_file
;
dyy_10.res created by SHELXL-2014/7
TITL DYY_10_a.res in P2(1)/c
REM Old TITL DYY_10 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.221, Rweak 0.007, Alpha 0.040, Orientation as input
REM Formula found by SHELXT: C54 Ni2
CELL 1.54178 19.2423 10.9261 21.5899 90 106.046 90
ZERR 4 0.0008 0.0005 0.001 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl F N Ni
UNIT 180 176 4 20 16 4
L.S. 10
PLAN 20
SIZE 0.11 0.15 0.26
TEMP -173.03
BOND $H
LIST 4
ABIN
fmap 2
acta
REM
REM
REM
WGHT 0.071500 1.596000
FVAR 0.08702
NI1 6 0.207429 0.390780 0.687832 11.00000 0.01931 0.02281 =
0.02494 -0.00071 0.00970 -0.00059
CL1 3 0.082221 0.381874 0.660820 11.00000 0.02084 0.02879 =
0.02870 0.00267 0.01007 0.00259
N2 5 0.283386 0.280079 0.745104 11.00000 0.01895 0.02134 =
0.02348 -0.00305 0.01056 0.00007
N1 5 0.276617 0.510830 0.663329 11.00000 0.02204 0.02082 =
0.02434 -0.00157 0.01011 -0.00095
F5 4 0.461397 0.272948 0.648076 11.00000 0.04610 0.09022 =
0.06118 -0.02560 0.02580 0.01092
F3 4 0.689446 0.384343 0.780291 11.00000 0.01660 0.08847 =
0.11273 0.06102 0.01824 0.00845
N4 5 0.207948 0.277859 0.603473 11.00000 0.02529 0.02287 =
0.02748 0.00044 0.01149 -0.00063
N3 5 0.209793 0.503927 0.772322 11.00000 0.02854 0.02115 =
0.02541 0.00032 0.01246 0.00076
F1 4 0.480224 0.519181 0.829172 11.00000 0.03879 0.09870 =
0.08461 -0.05946 0.00370 -0.00444
F4 4 0.606960 0.266182 0.675055 11.00000 0.05470 0.12508 =
0.10731 0.00878 0.05514 0.03806
F2 4 0.626034 0.510211 0.856572 11.00000 0.03323 0.11528 =
0.11920 -0.03093 -0.01198 -0.02120
C6 1 0.357037 0.300787 0.752039 11.00000 0.01991 0.02294 =
0.02849 -0.00279 0.01164 0.00031
C21 1 0.193553 0.667143 0.593280 11.00000 0.02325 0.01880 =
0.02233 -0.00034 0.01077 -0.00259
C5 1 0.266439 0.612570 0.626682 11.00000 0.02533 0.02174 =
0.02433 -0.00267 0.01190 -0.00139
C2 1 0.351382 0.491624 0.684563 11.00000 0.01931 0.02458 =
0.02891 -0.00312 0.01051 -0.00341
C25 1 0.129435 0.836517 0.518675 11.00000 0.03303 0.02131 =
0.02783 0.00439 0.01199 -0.00101
AFIX 13
H25 2 0.137058 0.909460 0.493349 11.00000 -1.20000
AFIX 0
C1 1 0.385785 0.396485 0.723976 11.00000 0.02377 0.02338 =
0.02917 -0.00446 0.01197 -0.00118
C9 1 0.279390 0.181284 0.781250 11.00000 0.02309 0.02088 =
0.02366 -0.00462 0.01172 0.00102
C29 1 0.072661 0.630133 0.511736 11.00000 0.02731 0.02170 =
0.02276 -0.00209 0.00753 -0.00174
AFIX 13
H29 2 0.042600 0.568078 0.482056 11.00000 -1.20000
AFIX 0
C7 1 0.398339 0.210719 0.794092 11.00000 0.02034 0.02826 =
0.03509 0.00036 0.00939 0.00378
AFIX 43
H7 2 0.449529 0.203438 0.807007 11.00000 -1.20000
AFIX 0
C24 1 0.202990 0.780797 0.553914 11.00000 0.02888 0.02437 =
0.02801 0.00026 0.01227 -0.00397
AFIX 23
H24A 2 0.232491 0.842705 0.583150 11.00000 -1.20000
H24B 2 0.229004 0.757262 0.522057 11.00000 -1.20000
AFIX 0
C23 1 0.146314 0.574212 0.545951 11.00000 0.02638 0.02111 =
0.02416 -0.00301 0.01127 -0.00162
AFIX 23
H23A 2 0.171352 0.549525 0.513562 11.00000 -1.20000
H23B 2 0.139155 0.500105 0.569850 11.00000 -1.20000
AFIX 0
C30 1 0.083419 0.741736 0.472965 11.00000 0.02779 0.02812 =
0.02435 0.00141 0.00833 -0.00109
AFIX 23
H30A 2 0.035916 0.777632 0.450440 11.00000 -1.20000
H30B 2 0.107912 0.717163 0.440168 11.00000 -1.20000
AFIX 0
C31 1 0.210721 0.126423 0.790043 11.00000 0.02581 0.02009 =
0.02763 0.00070 0.01434 0.00045
C34 1 0.170444 0.222183 0.819806 11.00000 0.02845 0.02265 =
0.03147 -0.00076 0.01472 0.00189
AFIX 23
H34A 2 0.202462 0.251049 0.861415 11.00000 -1.20000
H34B 2 0.157480 0.293506 0.790602 11.00000 -1.20000
AFIX 0
C27 1 0.079524 0.764505 0.607554 11.00000 0.02797 0.02398 =
0.02474 -0.00025 0.01198 0.00220
AFIX 13
H27 2 0.053976 0.789965 0.639996 11.00000 -1.20000
AFIX 0
C26 1 0.090415 0.876091 0.568411 11.00000 0.02939 0.02315 =
0.03037 -0.00052 0.00807 0.00039
AFIX 23
H26A 2 0.119479 0.938632 0.597507 11.00000 -1.20000
H26B 2 0.042963 0.912532 0.546206 11.00000 -1.20000
AFIX 0
C8 1 0.350167 0.136635 0.812349 11.00000 0.02636 0.02553 =
0.03228 0.00359 0.01023 0.00216
AFIX 43
H8 2 0.361674 0.068215 0.840484 11.00000 -1.20000
AFIX 0
C22 1 0.153103 0.708128 0.642354 11.00000 0.02600 0.02229 =
0.02356 -0.00225 0.01064 -0.00090
AFIX 23
H22A 2 0.145716 0.636773 0.668077 11.00000 -1.20000
H22B 2 0.182647 0.769115 0.672209 11.00000 -1.20000
AFIX 0
C4 1 0.334098 0.660448 0.623549 11.00000 0.02642 0.02609 =
0.03870 0.00362 0.01383 -0.00410
AFIX 43
H4 2 0.341221 0.731624 0.600779 11.00000 -1.20000
AFIX 0
C11 1 0.466729 0.395124 0.738454 11.00000 0.02055 0.02623 =
0.04136 0.00583 0.01182 0.00044
C3 1 0.386780 0.585822 0.659079 11.00000 0.02055 0.03230 =
0.03891 0.00105 0.01223 -0.00290
AFIX 43
H3 2 0.437412 0.594755 0.665646 11.00000 -1.20000
AFIX 0
C28 1 0.034266 0.668158 0.562377 11.00000 0.02231 0.02418 =
0.02975 0.00234 0.01060 -0.00008
AFIX 23
H28A 2 -0.014008 0.702176 0.540659 11.00000 -1.20000
H28B 2 0.027512 0.595667 0.587608 11.00000 -1.20000
AFIX 0
C35 1 0.101533 0.166005 0.830676 11.00000 0.03464 0.02792 =
0.04284 0.00383 0.02686 0.00363
AFIX 13
H35 2 0.076040 0.229487 0.849624 11.00000 -1.20000
AFIX 0
C32 1 0.228822 0.016089 0.836886 11.00000 0.03135 0.02719 =
0.03618 0.00580 0.01832 0.00719
AFIX 23
H32A 2 0.254441 -0.047307 0.818870 11.00000 -1.20000
H32B 2 0.261234 0.043123 0.878705 11.00000 -1.20000
AFIX 0
C41 1 0.151134 0.536083 0.789849 11.00000 0.03220 0.02776 =
0.03090 0.00123 0.01293 0.00809
AFIX 43
H41 2 0.105094 0.512201 0.763177 11.00000 -1.20000
AFIX 0
C37 1 0.159798 -0.038278 0.847446 11.00000 0.04179 0.02670 =
0.04531 0.00931 0.02637 0.00488
AFIX 13
H37 2 0.172869 -0.109286 0.877660 11.00000 -1.20000
AFIX 0
C45 1 0.274021 0.539338 0.810223 11.00000 0.03184 0.03751 =
0.03417 -0.00782 0.01507 -0.00469
AFIX 43
H45 2 0.316358 0.518426 0.798089 11.00000 -1.20000
AFIX 0
C46 1 0.148600 0.235235 0.560994 11.00000 0.02900 0.02416 =
0.03717 -0.00521 0.00509 0.00226
AFIX 43
H46 2 0.102936 0.251589 0.568124 11.00000 -1.20000
AFIX 0
C42 1 0.154145 0.602652 0.845098 11.00000 0.04604 0.03528 =
0.03261 -0.00154 0.01918 0.01163
AFIX 43
H42 2 0.111045 0.624373 0.855751 11.00000 -1.20000
AFIX 0
C33 1 0.160044 0.080772 0.725969 11.00000 0.02900 0.02782 =
0.03090 -0.00281 0.01329 -0.00343
AFIX 23
H33A 2 0.185114 0.017794 0.707131 11.00000 -1.20000
H33B 2 0.147325 0.149727 0.695155 11.00000 -1.20000
AFIX 0
C36 1 0.121093 0.058332 0.877044 11.00000 0.04008 0.03429 =
0.04452 0.00868 0.02762 0.00550
AFIX 23
H36A 2 0.076759 0.023058 0.884616 11.00000 -1.20000
H36B 2 0.153057 0.086113 0.918910 11.00000 -1.20000
AFIX 0
C39 1 0.090626 0.026028 0.736936 11.00000 0.03294 0.03075 =
0.04258 -0.00319 0.01485 -0.00888
AFIX 13
H39 2 0.057971 -0.002180 0.694844 11.00000 -1.20000
AFIX 0
C43 1 0.220226 0.636623 0.884090 11.00000 0.05599 0.03036 =
0.02887 -0.00393 0.02077 0.00335
AFIX 43
H43 2 0.223797 0.681082 0.922661 11.00000 -1.20000
AFIX 0
C44 1 0.281352 0.605431 0.866591 11.00000 0.04192 0.04245 =
0.03242 -0.00982 0.01445 -0.01119
AFIX 43
H44 2 0.327834 0.628691 0.892617 11.00000 -1.20000
AFIX 0
C48 1 0.215906 0.144370 0.495516 11.00000 0.05116 0.02493 =
0.02521 -0.00138 0.01344 0.00258
AFIX 43
H48 2 0.218348 0.099134 0.458598 11.00000 -1.20000
AFIX 0
C16 1 0.501307 0.332159 0.699984 11.00000 0.02986 0.04380 =
0.04930 0.00609 0.02061 0.00516
C38 1 0.110097 -0.082654 0.783296 11.00000 0.03705 0.02624 =
0.05834 -0.00128 0.02758 -0.00441
AFIX 23
H38A 2 0.065592 -0.118584 0.790189 11.00000 -1.20000
H38B 2 0.134834 -0.146541 0.764726 11.00000 -1.20000
AFIX 0
C40 1 0.051763 0.123840 0.766295 11.00000 0.02494 0.03281 =
0.05378 0.00877 0.02012 -0.00172
AFIX 23
H40A 2 0.038700 0.194373 0.736556 11.00000 -1.20000
H40B 2 0.006733 0.089374 0.772831 11.00000 -1.20000
AFIX 0
C47 1 0.150524 0.168686 0.507342 11.00000 0.03825 0.02861 =
0.03687 -0.00919 -0.00105 0.00443
AFIX 43
H47 2 0.106906 0.139648 0.478585 11.00000 -1.20000
AFIX 0
C12 1 0.510843 0.455603 0.791084 11.00000 0.02577 0.04041 =
0.05903 -0.00714 0.00842 -0.00505
C14 1 0.617334 0.387928 0.766577 11.00000 0.02062 0.04976 =
0.08177 0.03793 0.01825 0.00599
C50 1 0.270569 0.253308 0.591789 11.00000 0.03002 0.05937 =
0.03878 -0.02025 0.01384 -0.00537
AFIX 43
H50 2 0.313546 0.282394 0.621467 11.00000 -1.20000
AFIX 0
C49 1 0.276950 0.187178 0.538383 11.00000 0.03960 0.05915 =
0.04061 -0.01816 0.02207 -0.00477
AFIX 43
H49 2 0.323125 0.172244 0.532015 11.00000 -1.20000
AFIX 0
C13 1 0.585005 0.452155 0.805379 11.00000 0.02583 0.05077 =
0.07003 0.00698 0.00036 -0.01101
C15 1 0.575417 0.327735 0.713777 11.00000 0.03264 0.05826 =
0.06968 0.02286 0.03320 0.01636
HKLF 4
REM DYY_10_a.res in P2(1)/c
REM R1 = 0.0443 for 6417 Fo > 4sig(Fo) and 0.0526 for all 7681 data
REM 505 parameters refined using 0 restraints
END
WGHT 0.0714 1.5944
REM Highest difference peak 0.508, deepest hole -0.657, 1-sigma level 0.058
Q1 1 0.0615 0.3125 0.6505 11.00000 0.05 0.51
Q2 1 0.2252 0.4869 0.6700 11.00000 0.05 0.49
Q3 1 0.2037 0.2946 0.7081 11.00000 0.05 0.44
Q4 1 0.1504 0.3926 0.6973 11.00000 0.05 0.41
Q5 1 0.4666 0.2165 0.6798 11.00000 0.05 0.37
Q6 1 0.2013 0.4828 0.7028 11.00000 0.05 0.37
Q7 1 0.2025 0.7188 0.5754 11.00000 0.05 0.33
Q8 1 0.4630 0.5617 0.8128 11.00000 0.05 0.32
Q9 1 0.1398 0.3872 0.6548 11.00000 0.05 0.31
Q10 1 0.0981 0.4778 0.6446 11.00000 0.05 0.30
Q11 1 0.3194 0.2921 0.7503 11.00000 0.05 0.30
Q12 1 0.6176 0.5735 0.8401 11.00000 0.05 0.29
Q13 1 0.6039 0.2180 0.7009 11.00000 0.05 0.29
Q14 1 0.1897 0.1731 0.8000 11.00000 0.05 0.29
Q15 1 0.2623 0.3951 0.6811 11.00000 0.05 0.28
Q16 1 0.2635 0.3208 0.7282 11.00000 0.05 0.28
Q17 1 0.0768 0.4784 0.6813 11.00000 0.05 0.28
Q18 1 0.1151 0.1222 0.8565 11.00000 0.05 0.27
Q19 1 0.0752 0.6839 0.4929 11.00000 0.05 0.27
Q20 1 0.1128 0.7357 0.6192 11.00000 0.05 0.26
;
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14 2 11 0.2332 0.0000
14 2 12 0.0312 0.0000
14 2 13 0.1671 0.0000
14 2 14 -0.0752 0.0000
14 3 0 -0.9333 0.0000
14 3 1 0.1986 0.0000
14 3 2 0.8049 0.0000
14 3 3 0.2741 0.0000
14 3 4 1.6033 0.0000
14 3 5 -0.3426 0.0000
14 3 6 1.9518 0.0000
14 3 7 -0.8819 0.0000
14 3 8 1.9987 0.0000
14 3 9 -0.4745 0.0000
14 3 10 1.0179 0.0000
14 3 11 0.4150 0.0000
14 3 12 -0.4670 0.0000
14 3 13 0.7504 0.0000
14 3 14 -1.0002 0.0000
14 4 0 -3.9446 0.0000
14 4 1 -0.2815 0.0000
14 4 2 -3.1637 0.0000
14 4 3 0.2289 0.0000
14 4 4 -2.2095 0.0000
14 4 5 0.3962 0.0000
14 4 6 -1.7197 0.0000
14 4 7 0.0108 0.0000
14 4 8 -1.0736 0.0000
14 4 9 -0.5629 0.0000
14 4 10 -0.3347 0.0000
14 4 11 -0.7245 0.0000
14 4 12 -0.3717 0.0000
14 4 13 -0.3787 0.0000
14 5 0 0.2201 0.0000
14 5 1 0.0075 0.0000
14 5 2 0.0080 0.0000
14 5 3 -0.0200 0.0000
14 5 4 0.2219 0.0000
14 5 5 -0.1503 0.0000
14 5 6 0.8307 0.0000
14 5 7 -0.2731 0.0000
14 5 8 1.0447 0.0000
14 5 9 -0.6500 0.0000
14 5 10 0.7294 0.0000
14 5 11 -0.9045 0.0000
14 5 12 0.3400 0.0000
14 6 0 -1.9447 0.0000
14 6 1 0.0141 0.0000
14 6 2 -2.0150 0.0000
14 6 3 0.1798 0.0000
14 6 4 -1.9096 0.0000
14 6 5 0.2629 0.0000
14 6 6 -1.4046 0.0000
14 6 7 1.0566 0.0000
14 6 8 -0.8124 0.0000
14 6 9 1.4586 0.0000
14 6 10 -0.6445 0.0000
14 6 11 0.7149 0.0000
14 7 0 -0.8377 0.0000
14 7 1 -0.3165 0.0000
14 7 2 -0.4725 0.0000
14 7 3 0.2165 0.0000
14 7 4 0.2675 0.0000
14 7 5 0.1427 0.0000
14 7 6 0.8649 0.0000
14 7 7 -0.0661 0.0000
14 7 8 0.8734 0.0000
14 7 9 -0.0867 0.0000
14 7 10 0.4535 0.0000
14 8 0 -0.4618 0.0000
14 8 1 0.6689 0.0000
14 8 2 -0.0229 0.0000
14 8 3 0.8457 0.0000
14 8 4 0.4699 0.0000
14 8 5 0.6032 0.0000
14 8 6 0.9824 0.0000
14 8 7 0.2089 0.0000
14 8 8 0.9102 0.0000
14 9 0 -0.0199 0.0000
14 9 1 0.5129 0.0000
14 9 2 0.4188 0.0000
14 9 3 0.8217 0.0000
14 9 4 0.3575 0.0000
14 9 5 0.9259 0.0000
14 10 0 -0.0727 0.0000
15 0 0 2.7581 0.0000
15 0 2 1.4417 0.0000
15 0 4 0.2614 0.0000
15 0 6 0.2039 0.0000
15 0 12 -0.5960 0.0000
15 0 14 -0.0576 0.0000
15 1 0 -0.1626 0.0000
15 1 1 2.8228 0.0000
15 1 2 -0.6500 0.0000
15 1 3 2.1425 0.0000
15 1 4 -1.3220 0.0000
15 1 5 1.2570 0.0000
15 1 6 -1.7363 0.0000
15 1 7 0.8348 0.0000
15 1 8 -1.5042 0.0000
15 1 9 0.3707 0.0000
15 1 10 -0.7961 0.0000
15 1 11 -0.2484 0.0000
15 1 12 -0.1608 0.0000
15 1 13 -0.4242 0.0000
15 2 0 1.6077 0.0000
15 2 1 -1.6923 0.0000
15 2 2 1.8230 0.0000
15 2 3 -0.6919 0.0000
15 2 4 1.5240 0.0000
15 2 5 0.0468 0.0000
15 2 6 0.8827 0.0000
15 2 7 -0.1204 0.0000
15 2 8 0.3319 0.0000
15 2 9 -0.6737 0.0000
15 2 10 0.1060 0.0000
15 2 11 -0.8248 0.0000
15 2 12 0.2582 0.0000
15 2 13 -0.5326 0.0000
15 3 0 0.0475 0.0000
15 3 1 0.2250 0.0000
15 3 2 -1.1064 0.0000
15 3 3 0.4396 0.0000
15 3 4 -1.5881 0.0000
15 3 5 0.8791 0.0000
15 3 6 -1.9366 0.0000
15 3 7 1.0041 0.0000
15 3 8 -2.0695 0.0000
15 3 9 0.4625 0.0000
15 3 10 -1.3728 0.0000
15 3 11 -0.2264 0.0000
15 3 12 -0.2944 0.0000
15 3 13 -0.3318 0.0000
15 4 0 3.9803 0.0000
15 4 1 -0.7094 0.0000
15 4 2 3.1971 0.0000
15 4 3 -0.9620 0.0000
15 4 4 2.2275 0.0000
15 4 5 -0.8226 0.0000
15 4 6 1.1879 0.0000
15 4 7 -0.7332 0.0000
15 4 8 0.1037 0.0000
15 4 9 -0.6173 0.0000
15 4 10 -0.3528 0.0000
15 4 11 -0.3466 0.0000
15 4 12 0.1110 0.0000
15 5 0 -0.8959 0.0000
15 5 1 0.7765 0.0000
15 5 2 -0.5453 0.0000
15 5 3 0.4755 0.0000
15 5 4 -0.3578 0.0000
15 5 5 0.2763 0.0000
15 5 6 -0.6502 0.0000
15 5 7 0.1753 0.0000
15 5 8 -0.9555 0.0000
15 5 9 0.1368 0.0000
15 5 10 -0.8638 0.0000
15 5 11 0.0533 0.0000
15 6 0 2.4655 0.0000
15 6 1 -0.9150 0.0000
15 6 2 2.1134 0.0000
15 6 3 -1.1431 0.0000
15 6 4 1.4625 0.0000
15 6 5 -1.3460 0.0000
15 6 6 0.6685 0.0000
15 6 7 -1.6732 0.0000
15 6 8 0.2146 0.0000
15 6 9 -1.2922 0.0000
15 6 10 0.3132 0.0000
15 7 0 0.0728 0.0000
15 7 1 0.1854 0.0000
15 7 2 -0.4087 0.0000
15 7 3 -0.2035 0.0000
15 7 4 -0.8252 0.0000
15 7 5 -0.1388 0.0000
15 7 6 -0.9287 0.0000
15 7 7 -0.0523 0.0000
15 7 8 -0.7664 0.0000
15 8 0 -0.0913 0.0000
15 8 1 -0.9027 0.0000
15 8 2 -0.5496 0.0000
15 8 3 -0.8217 0.0000
15 8 4 -0.8612 0.0000
15 8 5 -0.3478 0.0000
15 8 6 -0.8636 0.0000
15 9 0 -0.3296 0.0000
15 9 1 -0.5921 0.0000
15 9 2 -0.4395 0.0000
16 0 0 -1.9535 0.0000
16 0 2 -1.4283 0.0000
16 0 4 -0.8502 0.0000
16 0 6 -0.8119 0.0000
16 1 0 -0.0638 0.0000
16 1 1 -3.7737 0.0000
16 1 2 0.3392 0.0000
16 1 3 -3.0024 0.0000
16 1 4 0.8735 0.0000
16 1 5 -1.9303 0.0000
16 1 6 1.2881 0.0000
16 1 7 -1.0903 0.0000
16 1 8 1.0042 0.0000
16 2 0 -1.9679 0.0000
16 2 1 2.0180 0.0000
16 2 2 -1.8934 0.0000
16 2 3 1.4344 0.0000
16 2 4 -1.4941 0.0000
16 2 5 0.8506 0.0000
16 2 6 -0.8633 0.0000
16 2 7 0.8065 0.0000
16 2 8 -0.2217 0.0000
16 2 9 1.0273 0.0000
16 2 10 -0.0739 0.0000
16 2 11 0.9493 0.0000
16 2 12 -0.4208 0.0000
16 3 0 0.0514 0.0000
16 3 1 -0.7870 0.0000
16 3 2 0.7318 0.0000
16 3 3 -0.8884 0.0000
16 3 4 0.9971 0.0000
16 3 5 -0.7783 0.0000
16 3 6 1.2158 0.0000
16 3 7 -0.5979 0.0000
16 3 8 1.3830 0.0000
16 3 9 -0.2345 0.0000
16 3 10 1.1366 0.0000
16 3 11 0.1109 0.0000
16 4 0 -3.2144 0.0000
16 4 1 1.0637 0.0000
16 4 2 -2.6426 0.0000
16 4 3 1.1239 0.0000
16 4 4 -1.6457 0.0000
16 4 5 1.1530 0.0000
16 4 6 -0.3180 0.0000
16 4 7 1.5175 0.0000
16 4 8 0.6414 0.0000
16 4 9 1.4267 0.0000
16 4 10 0.6212 0.0000
16 4 11 0.7397 0.0000
16 5 0 1.2450 0.0000
16 5 1 -0.7833 0.0000
16 5 2 0.8985 0.0000
16 5 3 -0.4778 0.0000
16 5 4 0.3549 0.0000
16 5 5 -0.3582 0.0000
16 5 6 0.3502 0.0000
16 5 7 -0.0700 0.0000
16 5 8 0.6652 0.0000
16 5 9 0.3795 0.0000
16 6 0 -2.3958 0.0000
16 6 1 1.4149 0.0000
16 6 2 -1.6299 0.0000
16 6 3 1.6644 0.0000
16 6 4 -0.7663 0.0000
16 6 5 1.6117 0.0000
16 6 6 -0.1391 0.0000
16 6 7 1.2581 0.0000
16 6 8 0.0211 0.0000
16 7 0 0.2676 0.0000
16 7 1 -0.3693 0.0000
16 7 2 0.5919 0.0000
16 7 3 -0.2747 0.0000
16 7 4 0.5571 0.0000
16 7 5 -0.2566 0.0000
16 7 6 0.3610 0.0000
16 8 0 0.2952 0.0000
16 8 1 0.4556 0.0000
16 8 2 0.6598 0.0000
16 8 3 0.2189 0.0000
16 8 4 0.6528 0.0000
17 0 0 2.7392 0.0000
17 0 2 2.9233 0.0000
17 0 4 2.2509 0.0000
17 0 6 1.6528 0.0000
17 1 0 0.5633 0.0000
17 1 1 4.1116 0.0000
17 1 2 0.1895 0.0000
17 1 3 3.1589 0.0000
17 1 4 -0.4126 0.0000
17 1 5 1.7693 0.0000
17 1 6 -0.8996 0.0000
17 1 7 0.5774 0.0000
17 1 8 -0.5473 0.0000
17 2 0 1.8631 0.0000
17 2 1 -1.9145 0.0000
17 2 2 1.5639 0.0000
17 2 3 -1.8817 0.0000
17 2 4 1.1298 0.0000
17 2 5 -1.2727 0.0000
17 2 6 0.4465 0.0000
17 2 7 -0.7955 0.0000
17 2 8 -0.1549 0.0000
17 2 9 -0.6276 0.0000
17 2 10 -0.0295 0.0000
17 3 0 0.2144 0.0000
17 3 1 1.1578 0.0000
17 3 2 -0.1938 0.0000
17 3 3 0.8129 0.0000
17 3 4 -0.1280 0.0000
17 3 5 0.2900 0.0000
17 3 6 0.0197 0.0000
17 3 7 0.1527 0.0000
17 3 8 -0.1392 0.0000
17 3 9 0.0767 0.0000
17 3 10 -0.3700 0.0000
17 4 0 1.7745 0.0000
17 4 1 -0.8655 0.0000
17 4 2 1.4128 0.0000
17 4 3 -0.7934 0.0000
17 4 4 0.5626 0.0000
17 4 5 -1.0355 0.0000
17 4 6 -0.4498 0.0000
17 4 7 -1.4123 0.0000
17 4 8 -0.7962 0.0000
17 4 9 -1.0322 0.0000
17 5 0 -1.3605 0.0000
17 5 1 0.1965 0.0000
17 5 2 -1.0912 0.0000
17 5 3 0.3426 0.0000
17 5 4 -0.3191 0.0000
17 5 5 0.5381 0.0000
17 5 6 -0.0979 0.0000
17 5 7 0.1234 0.0000
17 5 8 -0.2985 0.0000
17 6 0 1.5141 0.0000
17 6 1 -1.6062 0.0000
17 6 2 0.6813 0.0000
17 6 3 -1.5652 0.0000
17 6 4 0.1329 0.0000
17 6 5 -0.9920 0.0000
17 6 6 -0.0115 0.0000
17 7 0 -0.3321 0.0000
17 7 1 0.4465 0.0000
17 7 2 -0.4046 0.0000
17 7 3 0.5575 0.0000
17 7 4 -0.0837 0.0000
17 8 0 -0.3582 0.0000
17 8 1 -0.0466 0.0000
18 0 0 -2.7643 0.0000
18 0 2 -2.6537 0.0000
18 0 4 -1.6103 0.0000
18 0 6 -0.9350 0.0000
18 1 0 -0.6708 0.0000
18 1 1 -2.8862 0.0000
18 1 2 -0.2146 0.0000
18 1 3 -1.8234 0.0000
18 1 4 0.5405 0.0000
18 1 5 -0.4346 0.0000
18 1 6 0.9310 0.0000
18 1 7 0.5295 0.0000
18 1 8 0.4188 0.0000
18 2 0 -0.4740 0.0000
18 2 1 1.6823 0.0000
18 2 2 -0.1143 0.0000
18 2 3 1.6957 0.0000
18 2 4 0.2181 0.0000
18 2 5 0.7847 0.0000
18 2 6 0.6385 0.0000
18 2 7 -0.0057 0.0000
18 2 8 0.6821 0.0000
18 2 9 -0.2518 0.0000
18 3 0 -0.5445 0.0000
18 3 1 -0.8389 0.0000
18 3 2 -0.4251 0.0000
18 3 3 -0.1912 0.0000
18 3 4 -0.8570 0.0000
18 3 5 0.2260 0.0000
18 3 6 -1.1968 0.0000
18 3 7 0.0767 0.0000
18 3 8 -0.8492 0.0000
18 4 0 -0.2602 0.0000
18 4 1 0.3935 0.0000
18 4 2 -0.0793 0.0000
18 4 3 0.2033 0.0000
18 4 4 0.3984 0.0000
18 4 5 0.4033 0.0000
18 4 6 0.7607 0.0000
18 4 7 0.5015 0.0000
18 5 0 1.0933 0.0000
18 5 1 0.4243 0.0000
18 5 2 0.9330 0.0000
18 5 3 -0.1647 0.0000
18 5 4 0.1705 0.0000
18 5 5 -0.5398 0.0000
18 5 6 -0.0648 0.0000
18 6 0 -0.3353 0.0000
18 6 1 1.3897 0.0000
18 6 2 0.2088 0.0000
18 6 3 0.9752 0.0000
18 6 4 0.1996 0.0000
18 7 0 0.2962 0.0000
18 7 1 -0.1597 0.0000
19 0 0 0.9415 0.0000
19 0 2 0.2246 0.0000
19 0 4 -0.5558 0.0000
19 0 6 -0.4731 0.0000
19 1 0 0.4038 0.0000
19 1 1 0.8659 0.0000
19 1 2 -0.1528 0.0000
19 1 3 0.0962 0.0000
19 1 4 -0.8676 0.0000
19 1 5 -0.7341 0.0000
19 1 6 -0.9709 0.0000
19 1 7 -1.0012 0.0000
19 2 0 -1.0957 0.0000
19 2 1 -1.3559 0.0000
19 2 2 -1.3989 0.0000
19 2 3 -0.9703 0.0000
19 2 4 -1.5598 0.0000
19 2 5 0.0855 0.0000
19 2 6 -1.4238 0.0000
19 2 7 0.7420 0.0000
19 3 0 0.8772 0.0000
19 3 1 0.1825 0.0000
19 3 2 0.9854 0.0000
19 3 3 -0.3844 0.0000
19 3 4 1.4157 0.0000
19 3 5 -0.4288 0.0000
19 3 6 1.4906 0.0000
19 4 0 -0.4621 0.0000
19 4 1 -0.0854 0.0000
19 4 2 -0.4981 0.0000
19 4 3 0.1138 0.0000
19 4 4 -0.6655 0.0000
19 4 5 0.0871 0.0000
19 5 0 -0.5889 0.0000
19 5 1 -0.5911 0.0000
19 5 2 -0.5714 0.0000
19 5 3 0.0022 0.0000
19 5 4 -0.0145 0.0000
19 6 0 -0.3122 0.0000
19 6 1 -0.8326 0.0000
20 0 0 0.4903 0.0000
20 0 2 1.2728 0.0000
20 0 4 1.4090 0.0000
20 1 0 -0.2543 0.0000
20 1 1 -0.1149 0.0000
20 1 2 0.3093 0.0000
20 1 3 0.2311 0.0000
20 1 4 0.7846 0.0000
20 1 5 0.5160 0.0000
20 2 0 1.0861 0.0000
20 2 1 0.8397 0.0000
20 2 2 1.4563 0.0000
20 2 3 0.2755 0.0000
20 2 4 1.5848 0.0000
20 2 5 -0.4385 0.0000
20 3 0 -0.9745 0.0000
20 3 1 0.0941 0.0000
20 3 2 -1.0172 0.0000
20 3 3 0.4284 0.0000
20 3 4 -1.0547 0.0000
20 4 0 0.2029 0.0000
20 4 1 0.1233 0.0000
20 4 2 0.2162 0.0000
20 4 3 0.0182 0.0000
20 5 0 0.2668 0.0000
20 5 1 0.3557 0.0000
21 0 0 -0.0479 0.0000
21 0 2 -0.6364 0.0000
21 1 0 0.3573 0.0000
21 1 1 0.6908 0.0000
21 1 2 -0.0843 0.0000
21 1 3 0.4053 0.0000
21 2 0 0.1050 0.0000
21 2 1 -0.2992 0.0000
21 2 2 -0.4966 0.0000
21 3 0 0.5881 0.0000
21 3 1 -0.0201 0.0000
22 0 0 -0.7092 0.0000
0 0 0 0.0 0.0
_shelx_fab_checksum 12188
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_LNiNHAd
_database_code_depnum_ccdc_archive 'CCDC 1953733'
loop_
_audit_author_name
_audit_author_address
'Shao-Liang Zheng'
;Harvard Univerisity
United States of America
;
_audit_update_record
;
2019-09-16 deposited with the CCDC. 2019-12-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C45 H50 F5 N3 Ni'
_chemical_formula_weight 786.59
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.0799(4)
_cell_length_b 14.6404(5)
_cell_length_c 24.1769(10)
_cell_angle_alpha 90
_cell_angle_beta 91.408(2)
_cell_angle_gamma 90
_cell_volume 4274.5(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4358
_cell_measurement_theta_min 3.6575
_cell_measurement_theta_max 66.6225
_exptl_crystal_description plate
_exptl_crystal_colour pink
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.222
_exptl_crystal_F_000 1656
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.160
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.030
_exptl_absorpt_coefficient_mu 1.109
_shelx_estimated_absorpt_T_min 0.843
_shelx_estimated_absorpt_T_max 0.968
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6506
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details SADBAS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source 'I/mS microfocus tube'
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 44262
_diffrn_reflns_av_unetI/netI 0.0538
_diffrn_reflns_av_R_equivalents 0.0721
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 3.529
_diffrn_reflns_theta_max 66.671
_diffrn_reflns_theta_full 66.671
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.949
_reflns_number_total 7193
_reflns_number_gt 5315
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_cell_refinement 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_reduction 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. All non H-atoms were located in difference-Fourier maps, and then refined anisotropically. The disorder solvent could not be located in the Fourier map and have been squeezed out by using solvent mask from Olex2.
;
# start Validation Reply Form
_vrf_PLAT029_LNiNHAd
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.949 Why?
RESPONSE: The completeness is low due to geomertic limitation of Cu colletion.
;
# end Validation Reply Form
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.0531P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 7193
_refine_ls_number_parameters 490
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0595
_refine_ls_R_factor_gt 0.0392
_refine_ls_wR_factor_ref 0.0961
_refine_ls_wR_factor_gt 0.0890
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_restrained_S_all 1.032
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.49571(3) 0.51468(2) 0.74313(2) 0.02374(10) Uani 1 1 d . . . . .
F5 F 0.69755(10) 0.24599(9) 0.79991(5) 0.0334(3) Uani 1 1 d . . . . .
F1 F 0.93934(11) 0.49520(9) 0.82882(6) 0.0421(4) Uani 1 1 d . . . . .
F4 F 0.85787(12) 0.13049(10) 0.83435(6) 0.0458(4) Uani 1 1 d . . . . .
F2 F 1.10048(11) 0.37796(10) 0.86273(6) 0.0443(4) Uani 1 1 d . . . . .
F3 F 1.05968(11) 0.19587(11) 0.86553(6) 0.0497(4) Uani 1 1 d . . . . .
N1 N 0.64148(14) 0.51720(12) 0.71369(7) 0.0246(4) Uani 1 1 d . . . . .
N2 N 0.55070(14) 0.51401(12) 0.81810(7) 0.0246(4) Uani 1 1 d . . . . .
N3 N 0.36119(14) 0.49748(12) 0.71391(7) 0.0246(4) Uani 1 1 d . . . . .
C9 C 0.50392(17) 0.53880(14) 0.86604(9) 0.0247(5) Uani 1 1 d . . . . .
C5 C 0.68026(17) 0.54372(15) 0.66429(9) 0.0253(5) Uani 1 1 d . . . . .
C41 C 0.29922(17) 0.41439(15) 0.69968(9) 0.0243(5) Uani 1 1 d . . . . .
C1 C 0.72183(17) 0.43608(14) 0.79378(9) 0.0252(5) Uani 1 1 d . . . . .
C6 C 0.64339(18) 0.46137(15) 0.83208(9) 0.0267(5) Uani 1 1 d . . . . .
C31 C 0.40275(18) 0.59814(15) 0.86997(9) 0.0258(5) Uani 1 1 d . . . . .
C11 C 0.81296(17) 0.37446(15) 0.81393(9) 0.0263(5) Uani 1 1 d . . . . .
C21 C 0.61609(17) 0.60315(15) 0.62361(9) 0.0249(5) Uani 1 1 d . . . . .
C2 C 0.72543(17) 0.46491(15) 0.73904(9) 0.0260(5) Uani 1 1 d . . . . .
C16 C 0.79620(18) 0.28090(16) 0.81600(9) 0.0284(5) Uani 1 1 d . . . . .
C15 C 0.8772(2) 0.22092(16) 0.83335(10) 0.0331(5) Uani 1 1 d . . . . .
C43 C 0.36493(18) 0.33074(15) 0.71949(9) 0.0282(5) Uani 1 1 d . . . . .
H43A H 0.3775 0.3343 0.7601 0.034 Uiso 1 1 calc R U . . .
H43B H 0.4380 0.3301 0.7018 0.034 Uiso 1 1 calc R U . . .
C3 C 0.81596(17) 0.45864(15) 0.70310(9) 0.0283(5) Uani 1 1 d . . . . .
H3A H 0.8829 0.4259 0.7097 0.034 Uiso 1 1 calc R U . . .
C47 C 0.12237(18) 0.32582(16) 0.71307(9) 0.0304(5) Uani 1 1 d . . . . .
H47 H 0.0494 0.3262 0.7318 0.036 Uiso 1 1 calc R U . . .
C44 C 0.27867(19) 0.40766(17) 0.63684(9) 0.0309(5) Uani 1 1 d . . . . .
H44A H 0.2354 0.4612 0.6238 0.037 Uiso 1 1 calc R U . . .
H44B H 0.3504 0.4079 0.6179 0.037 Uiso 1 1 calc R U . . .
C22 C 0.56159(19) 0.68379(15) 0.65295(9) 0.0292(5) Uani 1 1 d . . . . .
H22A H 0.5109 0.6605 0.6812 0.035 Uiso 1 1 calc R U . . .
H22B H 0.6193 0.7211 0.6720 0.035 Uiso 1 1 calc R U . . .
C12 C 0.91698(18) 0.40542(16) 0.83031(9) 0.0307(5) Uani 1 1 d . . . . .
C27 C 0.4967(2) 0.74336(16) 0.61141(10) 0.0345(5) Uani 1 1 d . . . . .
H27 H 0.4612 0.7951 0.6313 0.041 Uiso 1 1 calc R U . . .
C8 C 0.56644(19) 0.50172(15) 0.91151(9) 0.0299(5) Uani 1 1 d . . . . .
H8 H 0.5516 0.5097 0.9496 0.036 Uiso 1 1 calc R U . . .
C45 C 0.21522(19) 0.31967(18) 0.62237(10) 0.0352(6) Uani 1 1 d . . . . .
H45 H 0.2031 0.3159 0.5814 0.042 Uiso 1 1 calc R U . . .
C35 C 0.3021(2) 0.73697(16) 0.83160(10) 0.0341(5) Uani 1 1 d . . . . .
H35 H 0.3049 0.7866 0.8033 0.041 Uiso 1 1 calc R U . . .
C49 C 0.30195(19) 0.24244(16) 0.70491(10) 0.0330(5) Uani 1 1 d . . . . .
H49 H 0.3462 0.1885 0.7178 0.040 Uiso 1 1 calc R U . . .
C7 C 0.65150(18) 0.45267(16) 0.89021(9) 0.0302(5) Uani 1 1 d . . . . .
H7 H 0.7059 0.4190 0.9106 0.036 Uiso 1 1 calc R U . . .
C50 C 0.2822(2) 0.23669(17) 0.64233(11) 0.0391(6) Uani 1 1 d . . . . .
H50A H 0.2413 0.1799 0.6330 0.047 Uiso 1 1 calc R U . . .
H50B H 0.3541 0.2350 0.6236 0.047 Uiso 1 1 calc R U . . .
C4 C 0.78862(18) 0.50873(16) 0.65715(9) 0.0291(5) Uani 1 1 d . . . . .
H4 H 0.8338 0.5184 0.6261 0.035 Uiso 1 1 calc R U . . .
C33 C 0.29605(18) 0.54150(16) 0.86030(10) 0.0322(5) Uani 1 1 d . . . . .
H33A H 0.2970 0.5130 0.8232 0.039 Uiso 1 1 calc R U . . .
H33B H 0.2928 0.4921 0.8882 0.039 Uiso 1 1 calc R U . . .
C42 C 0.18535(17) 0.41364(16) 0.72784(9) 0.0279(5) Uani 1 1 d . . . . .
H42A H 0.1964 0.4177 0.7685 0.033 Uiso 1 1 calc R U . . .
H42B H 0.1415 0.4673 0.7154 0.033 Uiso 1 1 calc R U . . .
C48 C 0.18998(19) 0.24284(16) 0.73315(10) 0.0340(5) Uani 1 1 d . . . . .
H48A H 0.2015 0.2459 0.7738 0.041 Uiso 1 1 calc R U . . .
H48B H 0.1492 0.1859 0.7241 0.041 Uiso 1 1 calc R U . . .
C23 C 0.52600(18) 0.54598(15) 0.59329(9) 0.0289(5) Uani 1 1 d . . . . .
H23A H 0.5609 0.4946 0.5736 0.035 Uiso 1 1 calc R U . . .
H23B H 0.4747 0.5202 0.6205 0.035 Uiso 1 1 calc R U . . .
C30 C 0.5401(2) 0.64420(17) 0.50883(9) 0.0348(5) Uani 1 1 d . . . . .
H30A H 0.5750 0.5933 0.4887 0.042 Uiso 1 1 calc R U . . .
H30B H 0.4983 0.6822 0.4816 0.042 Uiso 1 1 calc R U . . .
C24 C 0.69413(19) 0.64158(16) 0.57975(9) 0.0320(5) Uani 1 1 d . . . . .
H24A H 0.7297 0.5905 0.5601 0.038 Uiso 1 1 calc R U . . .
H24B H 0.7531 0.6784 0.5981 0.038 Uiso 1 1 calc R U . . .
C32 C 0.3981(2) 0.64143(16) 0.92774(9) 0.0341(5) Uani 1 1 d . . . . .
H32A H 0.3953 0.5926 0.9560 0.041 Uiso 1 1 calc R U . . .
H32B H 0.4659 0.6779 0.9349 0.041 Uiso 1 1 calc R U . . .
C14 C 0.97954(19) 0.25374(17) 0.84934(10) 0.0352(6) Uani 1 1 d . . . . .
C46 C 0.10251(18) 0.32005(17) 0.65078(10) 0.0341(5) Uani 1 1 d . . . . .
H46A H 0.0580 0.3730 0.6378 0.041 Uiso 1 1 calc R U . . .
H46B H 0.0612 0.2635 0.6413 0.041 Uiso 1 1 calc R U . . .
C34 C 0.40444(18) 0.67628(15) 0.82716(9) 0.0284(5) Uani 1 1 d . . . . .
H34A H 0.4719 0.7137 0.8334 0.034 Uiso 1 1 calc R U . . .
H34B H 0.4069 0.6501 0.7894 0.034 Uiso 1 1 calc R U . . .
C25 C 0.6288(2) 0.70160(16) 0.53782(10) 0.0340(5) Uani 1 1 d . . . . .
H25 H 0.6805 0.7263 0.5098 0.041 Uiso 1 1 calc R U . . .
C40 C 0.19830(19) 0.67860(18) 0.82106(10) 0.0378(6) Uani 1 1 d . . . . .
H40A H 0.1313 0.7173 0.8231 0.045 Uiso 1 1 calc R U . . .
H40B H 0.2002 0.6514 0.7836 0.045 Uiso 1 1 calc R U . . .
C13 C 0.99948(18) 0.34597(17) 0.84794(9) 0.0337(5) Uani 1 1 d . . . . .
C29 C 0.46109(19) 0.60599(16) 0.55170(9) 0.0321(5) Uani 1 1 d . . . . .
H29 H 0.4023 0.5686 0.5326 0.039 Uiso 1 1 calc R U . . .
C26 C 0.5751(2) 0.78091(17) 0.56847(10) 0.0373(6) Uani 1 1 d . . . . .
H26A H 0.6331 0.8186 0.5870 0.045 Uiso 1 1 calc R U . . .
H26B H 0.5336 0.8201 0.5418 0.045 Uiso 1 1 calc R U . . .
C36 C 0.3001(2) 0.77906(17) 0.88914(10) 0.0412(6) Uani 1 1 d . . . . .
H36A H 0.2343 0.8189 0.8923 0.049 Uiso 1 1 calc R U . . .
H36B H 0.3671 0.8169 0.8956 0.049 Uiso 1 1 calc R U . . .
C28 C 0.4073(2) 0.68523(18) 0.58252(10) 0.0371(6) Uani 1 1 d . . . . .
H28A H 0.3640 0.7234 0.5560 0.045 Uiso 1 1 calc R U . . .
H28B H 0.3561 0.6609 0.6103 0.045 Uiso 1 1 calc R U . . .
C37 C 0.2963(2) 0.70297(18) 0.93238(10) 0.0412(6) Uani 1 1 d . . . . .
H37 H 0.2951 0.7305 0.9702 0.049 Uiso 1 1 calc R U . . .
C39 C 0.1938(2) 0.60271(18) 0.86460(11) 0.0398(6) Uani 1 1 d . . . . .
H39 H 0.1253 0.5654 0.8583 0.048 Uiso 1 1 calc R U . . .
C38 C 0.1924(2) 0.6458(2) 0.92257(11) 0.0470(7) Uani 1 1 d . . . . .
H38A H 0.1260 0.6849 0.9258 0.056 Uiso 1 1 calc R U . . .
H38B H 0.1889 0.5972 0.9509 0.056 Uiso 1 1 calc R U . . .
H3 H 0.326(2) 0.548(2) 0.7039(11) 0.056 Uiso 1 1 d . U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01954(18) 0.0257(2) 0.0257(2) -0.00045(14) -0.00568(13) -0.00075(15)
F5 0.0296(7) 0.0313(8) 0.0388(8) 0.0006(5) -0.0079(5) -0.0040(6)
F1 0.0327(7) 0.0342(9) 0.0585(10) 0.0049(6) -0.0163(6) -0.0074(6)
F4 0.0438(9) 0.0272(8) 0.0658(11) 0.0047(6) -0.0104(7) 0.0051(6)
F2 0.0246(7) 0.0512(10) 0.0563(10) 0.0058(7) -0.0145(6) -0.0037(6)
F3 0.0339(8) 0.0475(10) 0.0669(11) 0.0095(7) -0.0123(7) 0.0145(7)
N1 0.0239(9) 0.0223(9) 0.0274(11) -0.0005(7) -0.0071(7) -0.0006(8)
N2 0.0227(9) 0.0236(9) 0.0274(11) 0.0003(7) -0.0048(7) -0.0014(8)
N3 0.0238(9) 0.0247(10) 0.0251(11) 0.0005(7) -0.0039(7) 0.0010(7)
C9 0.0244(11) 0.0234(12) 0.0261(13) -0.0015(8) -0.0029(9) -0.0042(9)
C5 0.0235(11) 0.0256(12) 0.0266(13) -0.0026(8) -0.0036(9) -0.0040(9)
C41 0.0221(11) 0.0262(12) 0.0243(13) -0.0018(8) -0.0040(8) -0.0021(9)
C1 0.0230(11) 0.0207(12) 0.0317(14) -0.0001(8) -0.0059(9) -0.0016(9)
C6 0.0252(11) 0.0244(12) 0.0301(14) 0.0023(8) -0.0067(9) -0.0013(9)
C31 0.0263(11) 0.0257(12) 0.0252(13) -0.0027(8) -0.0039(8) 0.0005(9)
C11 0.0237(11) 0.0314(13) 0.0235(13) 0.0028(8) -0.0032(8) 0.0007(9)
C21 0.0242(11) 0.0251(12) 0.0252(13) 0.0001(8) -0.0043(8) -0.0037(9)
C2 0.0231(11) 0.0263(12) 0.0282(13) -0.0002(8) -0.0071(8) -0.0007(9)
C16 0.0251(11) 0.0340(13) 0.0257(13) 0.0009(9) -0.0041(9) -0.0012(10)
C15 0.0353(13) 0.0264(13) 0.0373(15) 0.0033(9) -0.0046(10) 0.0024(10)
C43 0.0255(11) 0.0274(13) 0.0316(14) -0.0013(9) -0.0046(9) -0.0004(9)
C3 0.0208(11) 0.0312(13) 0.0327(14) -0.0013(9) -0.0028(9) 0.0027(9)
C47 0.0231(11) 0.0386(14) 0.0294(14) -0.0019(9) 0.0005(9) -0.0042(10)
C44 0.0280(12) 0.0402(14) 0.0244(13) 0.0005(9) -0.0020(9) -0.0057(10)
C22 0.0349(12) 0.0263(12) 0.0262(13) -0.0008(9) -0.0039(9) -0.0011(10)
C12 0.0296(12) 0.0298(13) 0.0324(14) 0.0028(9) -0.0037(9) -0.0039(10)
C27 0.0460(15) 0.0262(13) 0.0310(15) -0.0010(9) -0.0050(10) 0.0051(11)
C8 0.0332(12) 0.0338(14) 0.0226(13) 0.0026(9) -0.0033(9) -0.0014(10)
C45 0.0319(13) 0.0466(16) 0.0268(14) -0.0080(10) -0.0040(9) -0.0098(11)
C35 0.0387(13) 0.0317(13) 0.0318(15) -0.0006(9) -0.0034(10) 0.0066(11)
C49 0.0296(12) 0.0248(13) 0.0442(16) -0.0026(9) -0.0052(10) 0.0018(10)
C7 0.0299(12) 0.0329(13) 0.0273(14) 0.0059(9) -0.0078(9) 0.0001(10)
C50 0.0289(13) 0.0381(15) 0.0504(17) -0.0174(11) 0.0023(11) -0.0056(11)
C4 0.0245(11) 0.0341(13) 0.0286(13) 0.0019(9) 0.0004(9) -0.0013(10)
C33 0.0289(12) 0.0326(14) 0.0352(15) -0.0018(9) 0.0014(9) -0.0034(10)
C42 0.0223(11) 0.0339(13) 0.0272(14) -0.0012(9) -0.0019(9) 0.0021(9)
C48 0.0327(13) 0.0294(13) 0.0395(16) -0.0003(9) -0.0032(10) -0.0076(10)
C23 0.0304(12) 0.0282(12) 0.0276(14) -0.0019(9) -0.0055(9) -0.0033(10)
C30 0.0421(14) 0.0354(14) 0.0266(14) 0.0002(9) -0.0060(10) 0.0052(11)
C24 0.0308(12) 0.0343(14) 0.0308(14) 0.0034(9) -0.0016(9) -0.0044(10)
C32 0.0400(14) 0.0325(14) 0.0293(14) -0.0035(9) -0.0062(10) 0.0056(11)
C14 0.0296(12) 0.0379(15) 0.0378(16) 0.0067(10) -0.0048(10) 0.0093(10)
C46 0.0220(12) 0.0406(15) 0.0392(15) -0.0049(10) -0.0059(10) -0.0072(10)
C34 0.0296(12) 0.0265(12) 0.0290(13) -0.0002(9) -0.0039(9) -0.0008(9)
C25 0.0405(14) 0.0341(14) 0.0273(14) 0.0063(9) -0.0009(10) -0.0031(11)
C40 0.0277(12) 0.0473(16) 0.0382(15) -0.0057(11) -0.0035(10) 0.0112(11)
C13 0.0212(12) 0.0442(15) 0.0352(15) 0.0017(10) -0.0097(9) -0.0005(10)
C29 0.0350(13) 0.0353(14) 0.0255(14) -0.0014(9) -0.0110(9) -0.0009(10)
C26 0.0510(15) 0.0283(13) 0.0322(15) 0.0044(9) -0.0058(11) -0.0002(11)
C36 0.0466(15) 0.0333(15) 0.0433(17) -0.0081(11) -0.0073(11) 0.0109(12)
C28 0.0357(13) 0.0447(16) 0.0306(15) 0.0053(10) -0.0072(10) 0.0088(11)
C37 0.0487(15) 0.0459(16) 0.0290(15) -0.0100(10) 0.0000(11) 0.0125(12)
C39 0.0272(12) 0.0459(17) 0.0462(17) -0.0044(11) 0.0009(10) -0.0004(11)
C38 0.0431(15) 0.0554(18) 0.0432(18) 0.0037(12) 0.0142(12) 0.0167(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 1.7739(17) . ?
Ni1 N2 1.9149(17) . ?
Ni1 N1 1.9159(18) . ?
F5 C16 1.345(2) . ?
F1 C12 1.343(3) . ?
F4 C15 1.345(3) . ?
F2 C13 1.347(3) . ?
F3 C14 1.338(3) . ?
N1 C5 1.350(3) . ?
N1 C2 1.400(3) . ?
N2 C9 1.352(3) . ?
N2 C6 1.394(3) . ?
N3 C41 1.465(3) . ?
N3 H3 0.89(3) . ?
C9 C8 1.426(3) . ?
C9 C31 1.504(3) . ?
C5 C4 1.420(3) . ?
C5 C21 1.513(3) . ?
C41 C43 1.530(3) . ?
C41 C44 1.537(3) . ?
C41 C42 1.550(3) . ?
C1 C2 1.391(3) . ?
C1 C6 1.391(3) . ?
C1 C11 1.496(3) . ?
C6 C7 1.412(3) . ?
C31 C32 1.536(3) . ?
C31 C34 1.543(3) . ?
C31 C33 1.546(3) . ?
C11 C12 1.385(3) . ?
C11 C16 1.386(3) . ?
C21 C22 1.534(3) . ?
C21 C24 1.542(3) . ?
C21 C23 1.544(3) . ?
C2 C3 1.416(3) . ?
C16 C15 1.373(3) . ?
C15 C14 1.373(3) . ?
C43 C49 1.537(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C3 C4 1.365(3) . ?
C3 H3A 0.9500 . ?
C47 C46 1.521(3) . ?
C47 C42 1.532(3) . ?
C47 C48 1.536(3) . ?
C47 H47 1.0000 . ?
C44 C45 1.535(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C22 C27 1.531(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C12 C13 1.383(3) . ?
C27 C26 1.525(3) . ?
C27 C28 1.530(3) . ?
C27 H27 1.0000 . ?
C8 C7 1.365(3) . ?
C8 H8 0.9500 . ?
C45 C50 1.531(4) . ?
C45 C46 1.540(3) . ?
C45 H45 1.0000 . ?
C35 C36 1.522(3) . ?
C35 C34 1.529(3) . ?
C35 C40 1.533(3) . ?
C35 H35 1.0000 . ?
C49 C50 1.528(3) . ?
C49 C48 1.530(3) . ?
C49 H49 1.0000 . ?
C7 H7 0.9500 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C4 H4 0.9500 . ?
C33 C39 1.531(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C23 C29 1.536(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C30 C25 1.519(3) . ?
C30 C29 1.532(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C24 C25 1.544(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C32 C37 1.531(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C14 C13 1.372(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C25 C26 1.530(3) . ?
C25 H25 1.0000 . ?
C40 C39 1.532(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C29 C28 1.532(3) . ?
C29 H29 1.0000 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C36 C37 1.529(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C37 C38 1.522(4) . ?
C37 H37 1.0000 . ?
C39 C38 1.538(4) . ?
C39 H39 1.0000 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N2 132.02(8) . . ?
N3 Ni1 N1 134.11(8) . . ?
N2 Ni1 N1 92.93(7) . . ?
C5 N1 C2 106.33(17) . . ?
C5 N1 Ni1 132.54(14) . . ?
C2 N1 Ni1 119.30(14) . . ?
C9 N2 C6 106.90(17) . . ?
C9 N2 Ni1 131.88(14) . . ?
C6 N2 Ni1 119.36(14) . . ?
C41 N3 Ni1 132.01(14) . . ?
C41 N3 H3 112.7(19) . . ?
Ni1 N3 H3 115.1(19) . . ?
N2 C9 C8 109.53(19) . . ?
N2 C9 C31 124.51(18) . . ?
C8 C9 C31 125.9(2) . . ?
N1 C5 C4 110.16(18) . . ?
N1 C5 C21 123.85(19) . . ?
C4 C5 C21 126.0(2) . . ?
N3 C41 C43 109.45(16) . . ?
N3 C41 C44 110.77(17) . . ?
C43 C41 C44 109.16(18) . . ?
N3 C41 C42 110.90(17) . . ?
C43 C41 C42 108.43(18) . . ?
C44 C41 C42 108.07(17) . . ?
C2 C1 C6 126.2(2) . . ?
C2 C1 C11 116.94(19) . . ?
C6 C1 C11 116.84(19) . . ?
C1 C6 N2 122.81(19) . . ?
C1 C6 C7 127.3(2) . . ?
N2 C6 C7 109.08(19) . . ?
C9 C31 C32 110.11(17) . . ?
C9 C31 C34 111.21(18) . . ?
C32 C31 C34 107.78(18) . . ?
C9 C31 C33 110.88(18) . . ?
C32 C31 C33 108.04(19) . . ?
C34 C31 C33 108.72(17) . . ?
C12 C11 C16 116.5(2) . . ?
C12 C11 C1 123.5(2) . . ?
C16 C11 C1 120.06(19) . . ?
C5 C21 C22 111.16(18) . . ?
C5 C21 C24 110.17(18) . . ?
C22 C21 C24 108.28(18) . . ?
C5 C21 C23 109.94(17) . . ?
C22 C21 C23 109.35(17) . . ?
C24 C21 C23 107.88(17) . . ?
C1 C2 N1 122.92(19) . . ?
C1 C2 C3 127.4(2) . . ?
N1 C2 C3 109.19(19) . . ?
F5 C16 C15 117.7(2) . . ?
F5 C16 C11 119.63(19) . . ?
C15 C16 C11 122.7(2) . . ?
F4 C15 C16 120.8(2) . . ?
F4 C15 C14 119.7(2) . . ?
C16 C15 C14 119.5(2) . . ?
C41 C43 C49 110.58(17) . . ?
C41 C43 H43A 109.5 . . ?
C49 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C49 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
C4 C3 C2 106.8(2) . . ?
C4 C3 H3A 126.6 . . ?
C2 C3 H3A 126.6 . . ?
C46 C47 C42 110.04(19) . . ?
C46 C47 C48 109.80(19) . . ?
C42 C47 C48 109.45(18) . . ?
C46 C47 H47 109.2 . . ?
C42 C47 H47 109.2 . . ?
C48 C47 H47 109.2 . . ?
C45 C44 C41 110.29(18) . . ?
C45 C44 H44A 109.6 . . ?
C41 C44 H44A 109.6 . . ?
C45 C44 H44B 109.6 . . ?
C41 C44 H44B 109.6 . . ?
H44A C44 H44B 108.1 . . ?
C27 C22 C21 110.71(18) . . ?
C27 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C27 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
F1 C12 C13 118.7(2) . . ?
F1 C12 C11 119.6(2) . . ?
C13 C12 C11 121.6(2) . . ?
C26 C27 C28 109.4(2) . . ?
C26 C27 C22 109.6(2) . . ?
C28 C27 C22 109.07(19) . . ?
C26 C27 H27 109.6 . . ?
C28 C27 H27 109.6 . . ?
C22 C27 H27 109.6 . . ?
C7 C8 C9 107.4(2) . . ?
C7 C8 H8 126.3 . . ?
C9 C8 H8 126.3 . . ?
C50 C45 C44 109.70(19) . . ?
C50 C45 C46 109.2(2) . . ?
C44 C45 C46 109.7(2) . . ?
C50 C45 H45 109.4 . . ?
C44 C45 H45 109.4 . . ?
C46 C45 H45 109.4 . . ?
C36 C35 C34 109.28(19) . . ?
C36 C35 C40 110.3(2) . . ?
C34 C35 C40 108.90(19) . . ?
C36 C35 H35 109.5 . . ?
C34 C35 H35 109.5 . . ?
C40 C35 H35 109.5 . . ?
C50 C49 C48 108.88(19) . . ?
C50 C49 C43 109.75(19) . . ?
C48 C49 C43 109.42(19) . . ?
C50 C49 H49 109.6 . . ?
C48 C49 H49 109.6 . . ?
C43 C49 H49 109.6 . . ?
C8 C7 C6 107.1(2) . . ?
C8 C7 H7 126.5 . . ?
C6 C7 H7 126.5 . . ?
C49 C50 C45 109.69(19) . . ?
C49 C50 H50A 109.7 . . ?
C45 C50 H50A 109.7 . . ?
C49 C50 H50B 109.7 . . ?
C45 C50 H50B 109.7 . . ?
H50A C50 H50B 108.2 . . ?
C3 C4 C5 107.5(2) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
C39 C33 C31 110.29(19) . . ?
C39 C33 H33A 109.6 . . ?
C31 C33 H33A 109.6 . . ?
C39 C33 H33B 109.6 . . ?
C31 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C47 C42 C41 110.17(18) . . ?
C47 C42 H42A 109.6 . . ?
C41 C42 H42A 109.6 . . ?
C47 C42 H42B 109.6 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C49 C48 C47 109.33(19) . . ?
C49 C48 H48A 109.8 . . ?
C47 C48 H48A 109.8 . . ?
C49 C48 H48B 109.8 . . ?
C47 C48 H48B 109.8 . . ?
H48A C48 H48B 108.3 . . ?
C29 C23 C21 110.08(18) . . ?
C29 C23 H23A 109.6 . . ?
C21 C23 H23A 109.6 . . ?
C29 C23 H23B 109.6 . . ?
C21 C23 H23B 109.6 . . ?
H23A C23 H23B 108.2 . . ?
C25 C30 C29 109.50(18) . . ?
C25 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
C25 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
C21 C24 C25 110.34(19) . . ?
C21 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
C21 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C37 C32 C31 110.93(18) . . ?
C37 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C37 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
F3 C14 C13 120.3(2) . . ?
F3 C14 C15 120.1(2) . . ?
C13 C14 C15 119.7(2) . . ?
C47 C46 C45 108.79(18) . . ?
C47 C46 H46A 109.9 . . ?
C45 C46 H46A 109.9 . . ?
C47 C46 H46B 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
C35 C34 C31 111.08(19) . . ?
C35 C34 H34A 109.4 . . ?
C31 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C31 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C30 C25 C26 109.9(2) . . ?
C30 C25 C24 109.37(19) . . ?
C26 C25 C24 109.25(19) . . ?
C30 C25 H25 109.4 . . ?
C26 C25 H25 109.4 . . ?
C24 C25 H25 109.4 . . ?
C39 C40 C35 109.42(19) . . ?
C39 C40 H40A 109.8 . . ?
C35 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
C35 C40 H40B 109.8 . . ?
H40A C40 H40B 108.2 . . ?
F2 C13 C14 119.6(2) . . ?
F2 C13 C12 120.3(2) . . ?
C14 C13 C12 120.1(2) . . ?
C30 C29 C28 109.3(2) . . ?
C30 C29 C23 109.60(19) . . ?
C28 C29 C23 109.30(18) . . ?
C30 C29 H29 109.5 . . ?
C28 C29 H29 109.5 . . ?
C23 C29 H29 109.5 . . ?
C27 C26 C25 109.5(2) . . ?
C27 C26 H26A 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
C35 C36 C37 109.4(2) . . ?
C35 C36 H36A 109.8 . . ?
C37 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
C37 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
C27 C28 C29 109.90(19) . . ?
C27 C28 H28A 109.7 . . ?
C29 C28 H28A 109.7 . . ?
C27 C28 H28B 109.7 . . ?
C29 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C38 C37 C36 109.4(2) . . ?
C38 C37 C32 109.0(2) . . ?
C36 C37 C32 109.9(2) . . ?
C38 C37 H37 109.5 . . ?
C36 C37 H37 109.5 . . ?
C32 C37 H37 109.5 . . ?
C33 C39 C40 109.6(2) . . ?
C33 C39 C38 109.2(2) . . ?
C40 C39 C38 109.3(2) . . ?
C33 C39 H39 109.6 . . ?
C40 C39 H39 109.6 . . ?
C38 C39 H39 109.6 . . ?
C37 C38 C39 109.9(2) . . ?
C37 C38 H38A 109.7 . . ?
C39 C38 H38A 109.7 . . ?
C37 C38 H38B 109.7 . . ?
C39 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
_refine_diff_density_max 0.227
_refine_diff_density_min -0.265
_refine_diff_density_rms 0.044
_shelx_res_file
;
dyy_999.res created by SHELXL-2014/7
TITL DYY_999_a.res in P2(1)/c
REM Old TITL DYY_999 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.198, Rweak 0.008, Alpha 0.037, Orientation as input
REM Formula found by SHELXT: C55 Ni
CELL 1.54178 12.0799 14.6404 24.1769 90 91.408 90
ZERR 4 0.0004 0.0005 0.001 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N Ni
UNIT 180 200 20 12 4
L.S. 50
PLAN 20
SIZE 0.03 0.12 0.16
TEMP -173.12
BOND $H
LIST 4
ABIN
fmap 2
acta
REM
REM
REM
WGHT 0.037000 1.053100
FVAR 0.07757
NI1 5 0.495709 0.514682 0.743134 11.00000 0.01954 0.02567 =
0.02570 -0.00045 -0.00568 -0.00075
F5 3 0.697554 0.245990 0.799913 11.00000 0.02958 0.03134 =
0.03881 0.00057 -0.00786 -0.00403
F1 3 0.939338 0.495203 0.828817 11.00000 0.03267 0.03423 =
0.05852 0.00494 -0.01634 -0.00739
F4 3 0.857868 0.130486 0.834347 11.00000 0.04378 0.02715 =
0.06576 0.00468 -0.01036 0.00510
F2 3 1.100475 0.377957 0.862732 11.00000 0.02464 0.05116 =
0.05632 0.00581 -0.01450 -0.00370
F3 3 1.059678 0.195873 0.865528 11.00000 0.03390 0.04751 =
0.06694 0.00950 -0.01229 0.01452
N1 4 0.641480 0.517196 0.713686 11.00000 0.02386 0.02228 =
0.02742 -0.00053 -0.00710 -0.00061
N2 4 0.550704 0.514006 0.818096 11.00000 0.02267 0.02356 =
0.02735 0.00026 -0.00483 -0.00143
N3 4 0.361190 0.497484 0.713905 11.00000 0.02379 0.02475 =
0.02509 0.00046 -0.00386 0.00098
C9 1 0.503917 0.538799 0.866044 11.00000 0.02438 0.02339 =
0.02610 -0.00153 -0.00288 -0.00425
C5 1 0.680256 0.543718 0.664294 11.00000 0.02345 0.02557 =
0.02661 -0.00262 -0.00361 -0.00396
C41 1 0.299219 0.414391 0.699684 11.00000 0.02214 0.02623 =
0.02430 -0.00178 -0.00402 -0.00214
C1 1 0.721826 0.436080 0.793776 11.00000 0.02295 0.02067 =
0.03172 -0.00011 -0.00588 -0.00158
C6 1 0.643389 0.461371 0.832077 11.00000 0.02522 0.02444 =
0.03010 0.00231 -0.00669 -0.00135
C31 1 0.402753 0.598144 0.869970 11.00000 0.02631 0.02569 =
0.02517 -0.00268 -0.00387 0.00051
C11 1 0.812964 0.374455 0.813932 11.00000 0.02371 0.03140 =
0.02349 0.00284 -0.00318 0.00067
C21 1 0.616088 0.603149 0.623612 11.00000 0.02421 0.02506 =
0.02517 0.00014 -0.00431 -0.00365
C2 1 0.725434 0.464914 0.739045 11.00000 0.02315 0.02627 =
0.02823 -0.00018 -0.00705 -0.00074
C16 1 0.796201 0.280903 0.816000 11.00000 0.02515 0.03400 =
0.02573 0.00086 -0.00415 -0.00122
C15 1 0.877192 0.220924 0.833353 11.00000 0.03525 0.02640 =
0.03725 0.00326 -0.00457 0.00244
C43 1 0.364934 0.330744 0.719493 11.00000 0.02549 0.02739 =
0.03156 -0.00129 -0.00456 -0.00036
AFIX 23
H43A 2 0.377538 0.334269 0.760053 11.00000 -1.20000
H43B 2 0.438012 0.330068 0.701839 11.00000 -1.20000
AFIX 0
C3 1 0.815957 0.458636 0.703103 11.00000 0.02084 0.03124 =
0.03265 -0.00126 -0.00281 0.00265
AFIX 43
H3A 2 0.882852 0.425855 0.709709 11.00000 -1.20000
AFIX 0
C47 1 0.122366 0.325817 0.713068 11.00000 0.02307 0.03855 =
0.02943 -0.00194 0.00048 -0.00421
AFIX 13
H47 2 0.049441 0.326156 0.731767 11.00000 -1.20000
AFIX 0
C44 1 0.278670 0.407659 0.636842 11.00000 0.02802 0.04024 =
0.02436 0.00053 -0.00201 -0.00572
AFIX 23
H44A 2 0.235376 0.461235 0.623798 11.00000 -1.20000
H44B 2 0.350393 0.407908 0.617892 11.00000 -1.20000
AFIX 0
C22 1 0.561591 0.683785 0.652951 11.00000 0.03491 0.02633 =
0.02621 -0.00076 -0.00391 -0.00109
AFIX 23
H22A 2 0.510866 0.660464 0.681230 11.00000 -1.20000
H22B 2 0.619316 0.721080 0.671973 11.00000 -1.20000
AFIX 0
C12 1 0.916983 0.405424 0.830315 11.00000 0.02963 0.02975 =
0.03244 0.00279 -0.00368 -0.00390
C27 1 0.496709 0.743356 0.611410 11.00000 0.04600 0.02618 =
0.03096 -0.00103 -0.00499 0.00513
AFIX 13
H27 2 0.461206 0.795137 0.631300 11.00000 -1.20000
AFIX 0
C8 1 0.566436 0.501719 0.911511 11.00000 0.03319 0.03381 =
0.02262 0.00258 -0.00325 -0.00136
AFIX 43
H8 2 0.551612 0.509685 0.949616 11.00000 -1.20000
AFIX 0
C45 1 0.215221 0.319674 0.622372 11.00000 0.03187 0.04658 =
0.02684 -0.00798 -0.00398 -0.00979
AFIX 13
H45 2 0.203064 0.315919 0.581372 11.00000 -1.20000
AFIX 0
C35 1 0.302066 0.736969 0.831603 11.00000 0.03870 0.03170 =
0.03180 -0.00063 -0.00344 0.00664
AFIX 13
H35 2 0.304909 0.786633 0.803277 11.00000 -1.20000
AFIX 0
C49 1 0.301955 0.242442 0.704910 11.00000 0.02960 0.02479 =
0.04422 -0.00264 -0.00524 0.00177
AFIX 13
H49 2 0.346218 0.188459 0.717837 11.00000 -1.20000
AFIX 0
C7 1 0.651505 0.452667 0.890213 11.00000 0.02989 0.03291 =
0.02730 0.00585 -0.00784 0.00008
AFIX 43
H7 2 0.705908 0.419020 0.910640 11.00000 -1.20000
AFIX 0
C50 1 0.282179 0.236693 0.642333 11.00000 0.02886 0.03814 =
0.05042 -0.01744 0.00230 -0.00565
AFIX 23
H50A 2 0.241329 0.179921 0.632967 11.00000 -1.20000
H50B 2 0.354071 0.235032 0.623563 11.00000 -1.20000
AFIX 0
C4 1 0.788620 0.508732 0.657147 11.00000 0.02454 0.03408 =
0.02861 0.00194 0.00037 -0.00129
AFIX 43
H4 2 0.833806 0.518419 0.626076 11.00000 -1.20000
AFIX 0
C33 1 0.296046 0.541502 0.860300 11.00000 0.02886 0.03258 =
0.03520 -0.00182 0.00137 -0.00341
AFIX 23
H33A 2 0.296973 0.512980 0.823186 11.00000 -1.20000
H33B 2 0.292802 0.492139 0.888199 11.00000 -1.20000
AFIX 0
C42 1 0.185355 0.413642 0.727835 11.00000 0.02230 0.03393 =
0.02724 -0.00116 -0.00191 0.00213
AFIX 23
H42A 2 0.196413 0.417704 0.768471 11.00000 -1.20000
H42B 2 0.141456 0.467279 0.715422 11.00000 -1.20000
AFIX 0
C48 1 0.189981 0.242843 0.733154 11.00000 0.03274 0.02940 =
0.03954 -0.00029 -0.00320 -0.00760
AFIX 23
H48A 2 0.201497 0.245882 0.773796 11.00000 -1.20000
H48B 2 0.149220 0.185880 0.724144 11.00000 -1.20000
AFIX 0
C23 1 0.525998 0.545984 0.593288 11.00000 0.03042 0.02820 =
0.02764 -0.00186 -0.00548 -0.00330
AFIX 23
H23A 2 0.560947 0.494641 0.573584 11.00000 -1.20000
H23B 2 0.474726 0.520184 0.620529 11.00000 -1.20000
AFIX 0
C30 1 0.540076 0.644202 0.508833 11.00000 0.04205 0.03537 =
0.02662 0.00020 -0.00602 0.00520
AFIX 23
H30A 2 0.575046 0.593331 0.488703 11.00000 -1.20000
H30B 2 0.498261 0.682171 0.481638 11.00000 -1.20000
AFIX 0
C24 1 0.694128 0.641582 0.579754 11.00000 0.03076 0.03427 =
0.03080 0.00344 -0.00158 -0.00435
AFIX 23
H24A 2 0.729737 0.590535 0.560070 11.00000 -1.20000
H24B 2 0.753072 0.678436 0.598137 11.00000 -1.20000
AFIX 0
C32 1 0.398067 0.641432 0.927737 11.00000 0.04004 0.03253 =
0.02928 -0.00348 -0.00620 0.00556
AFIX 23
H32A 2 0.395294 0.592645 0.956023 11.00000 -1.20000
H32B 2 0.465932 0.677889 0.934918 11.00000 -1.20000
AFIX 0
C14 1 0.979536 0.253736 0.849337 11.00000 0.02957 0.03790 =
0.03776 0.00669 -0.00479 0.00932
C46 1 0.102508 0.320046 0.650784 11.00000 0.02200 0.04063 =
0.03925 -0.00494 -0.00589 -0.00719
AFIX 23
H46A 2 0.057999 0.373006 0.637828 11.00000 -1.20000
H46B 2 0.061157 0.263549 0.641348 11.00000 -1.20000
AFIX 0
C34 1 0.404437 0.676282 0.827161 11.00000 0.02963 0.02649 =
0.02895 -0.00025 -0.00391 -0.00078
AFIX 23
H34A 2 0.471902 0.713657 0.833366 11.00000 -1.20000
H34B 2 0.406948 0.650150 0.789446 11.00000 -1.20000
AFIX 0
C25 1 0.628761 0.701598 0.537821 11.00000 0.04050 0.03410 =
0.02735 0.00625 -0.00091 -0.00315
AFIX 13
H25 2 0.680457 0.726288 0.509811 11.00000 -1.20000
AFIX 0
C40 1 0.198296 0.678603 0.821058 11.00000 0.02774 0.04732 =
0.03818 -0.00572 -0.00353 0.01118
AFIX 23
H40A 2 0.131319 0.717314 0.823068 11.00000 -1.20000
H40B 2 0.200245 0.651397 0.783606 11.00000 -1.20000
AFIX 0
C13 1 0.999482 0.345967 0.847941 11.00000 0.02124 0.04421 =
0.03517 0.00171 -0.00968 -0.00054
C29 1 0.461094 0.605992 0.551697 11.00000 0.03497 0.03530 =
0.02546 -0.00141 -0.01105 -0.00092
AFIX 13
H29 2 0.402347 0.568619 0.532603 11.00000 -1.20000
AFIX 0
C26 1 0.575135 0.780907 0.568469 11.00000 0.05097 0.02834 =
0.03217 0.00444 -0.00582 -0.00022
AFIX 23
H26A 2 0.633148 0.818606 0.586955 11.00000 -1.20000
H26B 2 0.533580 0.820074 0.541818 11.00000 -1.20000
AFIX 0
C36 1 0.300119 0.779056 0.889135 11.00000 0.04656 0.03333 =
0.04329 -0.00808 -0.00730 0.01089
AFIX 23
H36A 2 0.234343 0.818887 0.892268 11.00000 -1.20000
H36B 2 0.367135 0.816890 0.895554 11.00000 -1.20000
AFIX 0
C28 1 0.407322 0.685229 0.582516 11.00000 0.03569 0.04469 =
0.03060 0.00528 -0.00719 0.00876
AFIX 23
H28A 2 0.364019 0.723433 0.556029 11.00000 -1.20000
H28B 2 0.356070 0.660912 0.610251 11.00000 -1.20000
AFIX 0
C37 1 0.296273 0.702970 0.932385 11.00000 0.04875 0.04586 =
0.02897 -0.01001 -0.00004 0.01252
AFIX 13
H37 2 0.295090 0.730468 0.970227 11.00000 -1.20000
AFIX 0
C39 1 0.193809 0.602711 0.864599 11.00000 0.02725 0.04594 =
0.04618 -0.00439 0.00092 -0.00045
AFIX 13
H39 2 0.125332 0.565368 0.858324 11.00000 -1.20000
AFIX 0
C38 1 0.192416 0.645845 0.922572 11.00000 0.04306 0.05543 =
0.04324 0.00374 0.01416 0.01674
AFIX 23
H38A 2 0.125997 0.684906 0.925833 11.00000 -1.20000
H38B 2 0.188904 0.597184 0.950909 11.00000 -1.20000
AFIX 0
H3 2 0.325555 0.548009 0.703868 11.00000 -1.20000
HKLF 4
REM DYY_999_a.res in P2(1)/c
REM R1 = 0.0392 for 5315 Fo > 4sig(Fo) and 0.0595 for all 7193 data
REM 490 parameters refined using 0 restraints
END
WGHT 0.0368 1.0656
REM Highest difference peak 0.227, deepest hole -0.265, 1-sigma level 0.044
Q1 1 0.4278 0.5122 0.6979 11.00000 0.05 0.23
Q2 1 0.5380 0.5780 0.7693 11.00000 0.05 0.22
Q3 1 1.0815 0.3907 0.9090 11.00000 0.05 0.22
Q4 1 0.5873 0.7390 0.5481 11.00000 0.05 0.21
Q5 1 0.4606 0.7136 0.5988 11.00000 0.05 0.21
Q6 1 0.2812 0.2560 0.6718 11.00000 0.05 0.20
Q7 1 0.2449 0.4075 0.7198 11.00000 0.05 0.20
Q8 1 0.5876 0.6370 0.6365 11.00000 0.05 0.19
Q9 1 0.7823 0.4806 0.7280 11.00000 0.05 0.19
Q10 1 0.5753 0.5773 0.6082 11.00000 0.05 0.19
Q11 1 0.6873 0.5004 0.7316 11.00000 0.05 0.19
Q12 1 0.2446 0.2756 0.6253 11.00000 0.05 0.18
Q13 1 0.3798 0.6154 0.8970 11.00000 0.05 0.18
Q14 1 0.1637 0.3166 0.6395 11.00000 0.05 0.18
Q15 1 0.8988 0.5197 0.8602 11.00000 0.05 0.18
Q16 1 0.6470 0.5727 0.6429 11.00000 0.05 0.17
Q17 1 0.6589 0.6776 0.5604 11.00000 0.05 0.17
Q18 1 0.5050 0.6306 0.7453 11.00000 0.05 0.17
Q19 1 0.4626 0.5752 0.7129 11.00000 0.05 0.17
Q20 1 0.9503 0.2248 0.8169 11.00000 0.05 0.17
;
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10 6 17 -0.3436 0.0000
10 7 0 0.1125 0.0000
10 7 1 1.5925 0.0000
10 7 2 0.7683 0.0000
10 7 3 1.5230 0.0000
10 7 4 1.6706 0.0000
10 7 5 1.5404 0.0000
10 7 6 2.1575 0.0000
10 7 7 1.1937 0.0000
10 7 8 2.0031 0.0000
10 7 9 0.2772 0.0000
10 7 10 1.5773 0.0000
10 7 11 -0.7629 0.0000
10 7 12 1.4319 0.0000
10 7 13 -1.2472 0.0000
10 7 14 1.6134 0.0000
10 7 15 -0.9977 0.0000
10 7 16 1.5981 0.0000
10 8 0 -1.3974 0.0000
10 8 1 -0.0756 0.0000
10 8 2 -1.3594 0.0000
10 8 3 -0.3416 0.0000
10 8 4 -1.1755 0.0000
10 8 5 -1.0849 0.0000
10 8 6 -1.0728 0.0000
10 8 7 -1.7685 0.0000
10 8 8 -0.6987 0.0000
10 8 9 -1.8262 0.0000
10 8 10 0.2603 0.0000
10 8 11 -1.1851 0.0000
10 8 12 1.3068 0.0000
10 8 13 -0.2931 0.0000
10 8 14 1.6014 0.0000
10 8 15 0.2116 0.0000
10 9 0 1.0105 0.0000
10 9 1 3.8012 0.0000
10 9 2 1.3505 0.0000
10 9 3 3.0492 0.0000
10 9 4 1.1864 0.0000
10 9 5 1.7604 0.0000
10 9 6 1.0428 0.0000
10 9 7 0.6479 0.0000
10 9 8 1.3335 0.0000
10 9 9 0.0537 0.0000
10 9 10 1.7069 0.0000
10 9 11 0.0263 0.0000
10 9 12 1.5837 0.0000
10 9 13 0.3867 0.0000
10 10 0 -0.7761 0.0000
10 10 1 -1.2300 0.0000
10 10 2 -0.9866 0.0000
10 10 3 -0.8184 0.0000
10 10 4 -0.8470 0.0000
10 10 5 -0.4568 0.0000
10 10 6 -0.3933 0.0000
10 10 7 -0.7037 0.0000
10 10 8 -0.0036 0.0000
10 10 9 -1.1407 0.0000
10 10 10 0.0492 0.0000
10 10 11 -0.9664 0.0000
10 11 0 1.5231 0.0000
10 11 1 1.2577 0.0000
10 11 2 1.2061 0.0000
10 11 3 0.3448 0.0000
10 11 4 0.9518 0.0000
10 11 5 -0.5330 0.0000
10 11 6 0.9506 0.0000
10 11 7 -0.9314 0.0000
10 11 8 1.1436 0.0000
10 11 9 -0.6512 0.0000
10 12 0 1.4749 0.0000
10 12 1 0.6981 0.0000
10 12 2 0.5433 0.0000
10 12 3 -0.5555 0.0000
10 12 4 -0.3424 0.0000
10 12 5 -1.2286 0.0000
11 0 0 -2.3967 0.0000
11 0 2 -4.2975 0.0000
11 0 4 -4.6068 0.0000
11 0 6 -3.5013 0.0000
11 0 10 -1.6894 0.0000
11 0 12 -0.9218 0.0000
11 0 14 -0.1138 0.0000
11 0 16 0.2449 0.0000
11 0 18 0.1513 0.0000
11 1 0 2.2943 0.0000
11 1 1 0.2737 0.0000
11 1 2 1.0841 0.0000
11 1 3 0.9309 0.0000
11 1 4 0.0620 0.0000
11 1 5 2.3232 0.0000
11 1 6 -0.1682 0.0000
11 1 7 2.4909 0.0000
11 1 8 0.2539 0.0000
11 1 9 0.7825 0.0000
11 1 10 0.7011 0.0000
11 1 11 -0.9537 0.0000
11 1 12 0.8133 0.0000
11 1 13 -1.1469 0.0000
11 1 14 0.7318 0.0000
11 1 15 -0.4544 0.0000
11 1 16 0.6589 0.0000
11 1 17 -0.1826 0.0000
11 2 0 -2.7572 0.0000
11 2 1 2.4386 0.0000
11 2 2 -3.8494 0.0000
11 2 3 2.1302 0.0000
11 2 4 -4.0765 0.0000
11 2 5 1.0377 0.0000
11 2 6 -3.4082 0.0000
11 2 7 -0.2943 0.0000
11 2 8 -2.5902 0.0000
11 2 9 -1.2952 0.0000
11 2 10 -1.7688 0.0000
11 2 11 -1.7560 0.0000
11 2 12 -0.7065 0.0000
11 2 13 -1.7628 0.0000
11 2 14 0.2575 0.0000
11 2 15 -1.4944 0.0000
11 2 16 0.5524 0.0000
11 2 17 -1.0436 0.0000
11 3 0 -1.3398 0.0000
11 3 1 0.9219 0.0000
11 3 2 -2.6828 0.0000
11 3 3 1.6626 0.0000
11 3 4 -3.4682 0.0000
11 3 5 2.7259 0.0000
11 3 6 -2.9588 0.0000
11 3 7 3.1575 0.0000
11 3 8 -1.7893 0.0000
11 3 9 2.6046 0.0000
11 3 10 -1.1946 0.0000
11 3 11 1.8083 0.0000
11 3 12 -1.3787 0.0000
11 3 13 1.2657 0.0000
11 3 14 -1.5097 0.0000
11 3 15 0.7365 0.0000
11 3 16 -1.0789 0.0000
11 3 17 0.1901 0.0000
11 4 0 0.2359 0.0000
11 4 1 2.9858 0.0000
11 4 2 0.2926 0.0000
11 4 3 1.9977 0.0000
11 4 4 0.7152 0.0000
11 4 5 0.1217 0.0000
11 4 6 1.3393 0.0000
11 4 7 -1.2247 0.0000
11 4 8 1.6350 0.0000
11 4 9 -1.2885 0.0000
11 4 10 1.5909 0.0000
11 4 11 -0.5615 0.0000
11 4 12 1.5096 0.0000
11 4 13 0.0265 0.0000
11 4 14 1.3080 0.0000
11 4 15 0.0464 0.0000
11 4 16 0.7567 0.0000
11 5 0 -2.8251 0.0000
11 5 1 0.9986 0.0000
11 5 2 -3.0461 0.0000
11 5 3 1.2727 0.0000
11 5 4 -2.5664 0.0000
11 5 5 0.8762 0.0000
11 5 6 -1.5412 0.0000
11 5 7 -0.1829 0.0000
11 5 8 -0.6982 0.0000
11 5 9 -1.3114 0.0000
11 5 10 -0.4892 0.0000
11 5 11 -1.8062 0.0000
11 5 12 -0.4952 0.0000
11 5 13 -1.5468 0.0000
11 5 14 -0.2307 0.0000
11 5 15 -0.8989 0.0000
11 5 16 0.0683 0.0000
11 6 0 0.9765 0.0000
11 6 1 0.1909 0.0000
11 6 2 1.8228 0.0000
11 6 3 0.1020 0.0000
11 6 4 2.6376 0.0000
11 6 5 -0.2899 0.0000
11 6 6 3.0896 0.0000
11 6 7 -0.1669 0.0000
11 6 8 3.0545 0.0000
11 6 9 0.3425 0.0000
11 6 10 2.7199 0.0000
11 6 11 0.4969 0.0000
11 6 12 2.1494 0.0000
11 6 13 0.1095 0.0000
11 6 14 1.2372 0.0000
11 6 15 -0.3394 0.0000
11 7 0 -0.6948 0.0000
11 7 1 -2.2724 0.0000
11 7 2 0.2612 0.0000
11 7 3 -2.0554 0.0000
11 7 4 1.2353 0.0000
11 7 5 -1.3202 0.0000
11 7 6 1.6207 0.0000
11 7 7 -0.8150 0.0000
11 7 8 1.2965 0.0000
11 7 9 -0.8934 0.0000
11 7 10 0.7385 0.0000
11 7 11 -1.1588 0.0000
11 7 12 0.5608 0.0000
11 7 13 -1.0417 0.0000
11 8 0 -0.9725 0.0000
11 8 1 -1.0770 0.0000
11 8 2 -0.7211 0.0000
11 8 3 -1.4880 0.0000
11 8 4 -0.4784 0.0000
11 8 5 -2.0972 0.0000
11 8 6 -0.2928 0.0000
11 8 7 -2.3356 0.0000
11 8 8 0.1882 0.0000
11 8 9 -1.8525 0.0000
11 8 10 0.9436 0.0000
11 8 11 -0.8452 0.0000
11 8 12 1.2893 0.0000
11 9 0 -1.0028 0.0000
11 9 1 2.5565 0.0000
11 9 2 -0.3642 0.0000
11 9 3 2.2706 0.0000
11 9 4 0.1271 0.0000
11 9 5 1.3650 0.0000
11 9 6 0.6561 0.0000
11 9 7 0.3389 0.0000
11 9 8 1.1431 0.0000
11 9 9 -0.2893 0.0000
11 9 10 1.2211 0.0000
11 10 0 -0.4687 0.0000
11 10 1 0.5619 0.0000
11 10 2 -0.2421 0.0000
11 10 3 1.5809 0.0000
11 10 4 0.0041 0.0000
11 10 5 1.7627 0.0000
11 10 6 0.1514 0.0000
11 10 7 0.8539 0.0000
11 11 0 1.6779 0.0000
11 11 1 1.6892 0.0000
11 11 2 1.0222 0.0000
11 11 3 1.2314 0.0000
12 0 0 -2.7799 0.0000
12 0 2 -4.1396 0.0000
12 0 4 -3.5611 0.0000
12 0 6 -1.9287 0.0000
12 1 0 0.6418 0.0000
12 1 1 -0.2514 0.0000
12 1 2 0.0678 0.0000
12 1 3 0.6676 0.0000
12 1 4 -0.2616 0.0000
12 1 5 2.5256 0.0000
12 1 6 -0.2980 0.0000
12 1 7 3.3147 0.0000
12 1 8 -0.2752 0.0000
12 2 0 -2.4298 0.0000
12 2 1 -0.0417 0.0000
12 2 2 -3.2399 0.0000
12 2 3 -0.9299 0.0000
12 2 4 -2.7692 0.0000
12 2 5 -1.9672 0.0000
12 2 6 -1.6780 0.0000
12 2 7 -2.7606 0.0000
12 2 8 -1.2213 0.0000
12 2 9 -3.0788 0.0000
12 2 10 -1.3969 0.0000
12 3 0 -0.5723 0.0000
12 3 1 1.4136 0.0000
12 3 2 -0.7325 0.0000
12 3 3 2.2250 0.0000
12 3 4 -0.2639 0.0000
12 3 5 3.3203 0.0000
12 3 6 0.6698 0.0000
12 3 7 3.5978 0.0000
12 3 8 1.0850 0.0000
12 3 9 2.8634 0.0000
12 3 10 0.4210 0.0000
12 3 11 1.9580 0.0000
12 3 12 -0.6251 0.0000
12 4 0 0.7080 0.0000
12 4 1 0.0535 0.0000
12 4 2 0.4050 0.0000
12 4 3 -1.2081 0.0000
12 4 4 0.6207 0.0000
12 4 5 -2.6176 0.0000
12 4 6 1.2467 0.0000
12 4 7 -3.0078 0.0000
12 4 8 1.6657 0.0000
12 4 9 -2.3026 0.0000
12 4 10 1.6585 0.0000
12 4 11 -1.2666 0.0000
12 4 12 1.3648 0.0000
12 4 13 -0.5219 0.0000
12 5 0 -0.5447 0.0000
12 5 1 -0.6478 0.0000
12 5 2 -0.2924 0.0000
12 5 3 -0.7757 0.0000
12 5 4 0.2713 0.0000
12 5 5 -1.1472 0.0000
12 5 6 0.9839 0.0000
12 5 7 -1.6600 0.0000
12 5 8 1.1858 0.0000
12 5 9 -1.9465 0.0000
12 5 10 0.7047 0.0000
12 5 11 -1.7314 0.0000
12 5 12 0.1813 0.0000
12 6 0 2.4728 0.0000
12 6 1 1.7815 0.0000
12 6 2 3.2305 0.0000
12 6 3 1.6816 0.0000
12 6 4 3.4074 0.0000
12 6 5 1.2083 0.0000
12 6 6 2.9879 0.0000
12 6 7 1.0349 0.0000
12 6 8 2.2355 0.0000
12 6 9 0.9247 0.0000
12 6 10 1.5091 0.0000
12 6 11 0.4717 0.0000
12 7 0 -0.0368 0.0000
12 7 1 -3.0028 0.0000
12 7 2 0.4971 0.0000
12 7 3 -3.1427 0.0000
12 7 4 0.8746 0.0000
12 7 5 -2.5033 0.0000
12 7 6 0.8730 0.0000
12 7 7 -1.6478 0.0000
12 7 8 0.3994 0.0000
12 7 9 -1.0153 0.0000
12 7 10 -0.2436 0.0000
12 8 0 -0.3297 0.0000
12 8 1 -0.8345 0.0000
12 8 2 -0.1843 0.0000
12 8 3 -0.7932 0.0000
12 8 4 -0.2127 0.0000
12 8 5 -0.8863 0.0000
12 8 6 -0.1833 0.0000
12 8 7 -0.8111 0.0000
12 8 8 0.2216 0.0000
12 9 0 -2.1395 0.0000
12 9 1 0.9655 0.0000
12 9 2 -1.6303 0.0000
12 9 3 0.7944 0.0000
12 9 4 -0.8649 0.0000
12 9 5 0.3531 0.0000
13 0 0 -0.4954 0.0000
13 0 2 -1.4519 0.0000
13 0 4 -1.0229 0.0000
13 1 0 -0.3798 0.0000
13 1 1 -0.7447 0.0000
13 1 2 -0.4695 0.0000
13 1 3 -0.8381 0.0000
13 1 4 -0.1822 0.0000
13 1 5 0.3331 0.0000
13 1 6 0.1313 0.0000
13 1 7 1.2965 0.0000
13 2 0 -1.6857 0.0000
13 2 1 -2.2228 0.0000
13 2 2 -2.2709 0.0000
13 2 3 -2.7896 0.0000
13 2 4 -1.5084 0.0000
13 2 5 -2.8652 0.0000
13 2 6 -0.3459 0.0000
13 2 7 -2.6556 0.0000
13 2 8 -0.0207 0.0000
13 2 9 -2.4010 0.0000
13 3 0 -0.5188 0.0000
13 3 1 1.0331 0.0000
13 3 2 -0.3545 0.0000
13 3 3 1.5781 0.0000
13 3 4 0.7389 0.0000
13 3 5 2.1928 0.0000
13 3 6 2.0165 0.0000
13 3 7 2.0438 0.0000
13 3 8 2.3132 0.0000
13 3 9 1.2765 0.0000
13 3 10 1.4087 0.0000
13 4 0 -0.6170 0.0000
13 4 1 -2.4112 0.0000
13 4 2 -1.1313 0.0000
13 4 3 -2.7353 0.0000
13 4 4 -0.8383 0.0000
13 4 5 -2.3576 0.0000
13 4 6 -0.0280 0.0000
13 4 7 -1.3500 0.0000
13 4 8 0.5399 0.0000
13 4 9 -0.4898 0.0000
13 5 0 0.4535 0.0000
13 5 1 -0.4654 0.0000
13 5 2 0.9366 0.0000
13 5 3 -0.4408 0.0000
13 5 4 1.6518 0.0000
13 5 5 -0.3921 0.0000
13 5 6 2.2046 0.0000
13 5 7 -0.3875 0.0000
13 5 8 1.9391 0.0000
13 6 0 1.4964 0.0000
13 6 1 1.4196 0.0000
13 6 2 1.7856 0.0000
13 6 3 1.0126 0.0000
13 6 4 1.5209 0.0000
13 6 5 0.7006 0.0000
13 6 6 0.8818 0.0000
13 7 0 0.3102 0.0000
13 7 1 -1.0914 0.0000
13 7 2 0.3124 0.0000
13 7 3 -1.3086 0.0000
14 0 0 1.2985 0.0000
14 0 2 0.3623 0.0000
14 0 4 -0.0748 0.0000
14 1 0 -0.3073 0.0000
14 1 1 -0.1351 0.0000
14 1 2 -0.4287 0.0000
14 1 3 -0.5262 0.0000
14 1 4 -0.2331 0.0000
14 1 5 -0.1722 0.0000
14 2 0 -0.8868 0.0000
14 2 1 -1.4009 0.0000
14 2 2 -1.3270 0.0000
14 2 3 -1.6202 0.0000
14 2 4 -0.9075 0.0000
14 2 5 -1.1537 0.0000
14 3 0 -1.0060 0.0000
14 3 1 0.6421 0.0000
14 3 2 -1.3312 0.0000
14 3 3 0.7681 0.0000
0 0 0 0.0 0.0
_shelx_fab_checksum 59366
;
#===END
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_LNiNMes
_database_code_depnum_ccdc_archive 'CCDC 1953731'
loop_
_audit_author_name
_audit_author_address
'Shao-Liang Zheng'
;Harvard Univerisity
United States of America
;
_audit_update_record
;
2019-09-16 deposited with the CCDC. 2019-12-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C44 H45 F5 N3 Ni'
_chemical_formula_weight 769.54
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.5949(7)
_cell_length_b 11.8426(10)
_cell_length_c 18.3253(14)
_cell_angle_alpha 92.953(3)
_cell_angle_beta 104.293(2)
_cell_angle_gamma 100.626(2)
_cell_volume 1972.9(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9938
_cell_measurement_theta_min 2.306
_cell_measurement_theta_max 25.022
_exptl_crystal_description plate
_exptl_crystal_colour pink
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.295
_exptl_crystal_F_000 806
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.030
_exptl_absorpt_coefficient_mu 0.549
_shelx_estimated_absorpt_T_min 0.870
_shelx_estimated_absorpt_T_max 0.984
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6482
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_process_details SADBAS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source 'fine-focus sealed tube'
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29313
_diffrn_reflns_av_unetI/netI 0.0575
_diffrn_reflns_av_R_equivalents 0.0591
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 2.199
_diffrn_reflns_theta_max 25.055
_diffrn_reflns_theta_full 25.055
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 6993
_reflns_number_gt 5464
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_cell_refinement 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_reduction 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. All non H-atoms were located in difference-Fourier maps, and then refined anisotropically. The disorder solvent could not be located in the Fourier map and have been squeezed out by using solvent mask from Olex2.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.7376P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6993
_refine_ls_number_parameters 481
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0722
_refine_ls_R_factor_gt 0.0517
_refine_ls_wR_factor_ref 0.1477
_refine_ls_wR_factor_gt 0.1334
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_restrained_S_all 1.044
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.50871(4) 0.44245(3) 0.26705(2) 0.01533(14) Uani 1 1 d . . . . .
F5 F 0.55661(18) 0.70803(16) 0.50161(10) 0.0262(4) Uani 1 1 d . . . . .
F3 F 0.3030(2) 1.00349(15) 0.52847(10) 0.0260(4) Uani 1 1 d . . . . .
F1 F 0.19586(19) 0.78419(15) 0.29445(10) 0.0266(4) Uani 1 1 d . . . . .
F4 F 0.50867(19) 0.88015(16) 0.58810(9) 0.0263(4) Uani 1 1 d . . . . .
F2 F 0.1446(2) 0.95319(16) 0.38291(10) 0.0293(5) Uani 1 1 d . . . . .
N1 N 0.5655(3) 0.6055(2) 0.26479(14) 0.0175(6) Uani 1 1 d . . . . .
N2 N 0.3237(2) 0.4495(2) 0.28586(13) 0.0135(5) Uani 1 1 d . . . . .
N3 N 0.6156(2) 0.3435(2) 0.28935(14) 0.0167(6) Uani 1 1 d . . . . .
C2 C 0.5254(3) 0.6817(3) 0.31323(16) 0.0163(6) Uani 1 1 d . . . . .
C1 C 0.4087(3) 0.6487(3) 0.34566(16) 0.0161(6) Uani 1 1 d . . . . .
C11 C 0.3781(3) 0.7402(2) 0.39516(16) 0.0160(6) Uani 1 1 d . . . . .
C5 C 0.6718(3) 0.6680(3) 0.23836(16) 0.0158(6) Uani 1 1 d . . . . .
C6 C 0.3128(3) 0.5420(3) 0.33343(16) 0.0160(6) Uani 1 1 d . . . . .
C9 C 0.2054(3) 0.3654(3) 0.28049(16) 0.0159(6) Uani 1 1 d . . . . .
C43 C 0.8609(3) 0.1636(3) 0.38481(17) 0.0184(7) Uani 1 1 d . . . . .
H43 H 0.8855 0.0909 0.3760 0.022 Uiso 1 1 calc R U . . .
C7 C 0.1850(3) 0.5097(3) 0.35905(16) 0.0178(7) Uani 1 1 d . . . . .
H7 H 0.1522 0.5554 0.3929 0.021 Uiso 1 1 calc R U . . .
C3 C 0.6132(3) 0.7923(3) 0.31688(18) 0.0208(7) Uani 1 1 d . . . . .
H3 H 0.6106 0.8600 0.3463 0.025 Uiso 1 1 calc R U . . .
C16 C 0.4544(3) 0.7677(3) 0.47084(17) 0.0175(7) Uani 1 1 d . . . . .
C15 C 0.4297(3) 0.8542(3) 0.51575(16) 0.0179(7) Uani 1 1 d . . . . .
C22 C 0.6216(3) 0.5326(3) 0.12096(17) 0.0184(7) Uani 1 1 d . . . . .
H22A H 0.5745 0.4688 0.1452 0.022 Uiso 1 1 calc R U . . .
H22B H 0.5449 0.5734 0.0954 0.022 Uiso 1 1 calc R U . . .
C4 C 0.7029(3) 0.7841(3) 0.27025(17) 0.0203(7) Uani 1 1 d . . . . .
H4 H 0.7734 0.8453 0.2609 0.024 Uiso 1 1 calc R U . . .
C31 C 0.1703(3) 0.2558(3) 0.22830(16) 0.0160(6) Uani 1 1 d . . . . .
C41 C 0.7141(3) 0.3060(3) 0.34363(17) 0.0166(6) Uani 1 1 d . . . . .
C42 C 0.7519(3) 0.1973(3) 0.33112(17) 0.0172(7) Uani 1 1 d . . . . .
C37 C -0.0303(3) 0.0883(3) 0.15891(18) 0.0229(7) Uani 1 1 d . . . . .
H37 H -0.1369 0.0529 0.1499 0.027 Uiso 1 1 calc R U . . .
C46 C 0.7841(3) 0.3759(3) 0.41364(16) 0.0174(7) Uani 1 1 d . . . . .
C14 C 0.3255(3) 0.9172(3) 0.48599(18) 0.0201(7) Uani 1 1 d . . . . .
C45 C 0.8951(3) 0.3380(3) 0.46516(17) 0.0202(7) Uani 1 1 d . . . . .
H45 H 0.9447 0.3853 0.5111 0.024 Uiso 1 1 calc R U . . .
C8 C 0.1175(3) 0.4008(3) 0.32619(17) 0.0188(7) Uani 1 1 d . . . . .
H8 H 0.0287 0.3570 0.3326 0.023 Uiso 1 1 calc R U . . .
C12 C 0.2732(3) 0.8053(3) 0.36741(16) 0.0185(7) Uani 1 1 d . . . . .
C21 C 0.7395(3) 0.6169(3) 0.18180(16) 0.0164(6) Uani 1 1 d . . . . .
C13 C 0.2467(3) 0.8914(3) 0.41137(17) 0.0200(7) Uani 1 1 d . . . . .
C35 C 0.1650(3) 0.1713(3) 0.09817(17) 0.0219(7) Uani 1 1 d . . . . .
H35 H 0.1871 0.1898 0.0491 0.026 Uiso 1 1 calc R U . . .
C32 C 0.0074(3) 0.1984(3) 0.21348(17) 0.0197(7) Uani 1 1 d . . . . .
H32A H -0.0145 0.1792 0.2619 0.024 Uiso 1 1 calc R U . . .
H32B H -0.0542 0.2531 0.1917 0.024 Uiso 1 1 calc R U . . .
C23 C 0.8587(3) 0.5529(3) 0.22065(17) 0.0188(7) Uani 1 1 d . . . . .
H23A H 0.8151 0.4898 0.2466 0.023 Uiso 1 1 calc R U . . .
H23B H 0.9362 0.6070 0.2592 0.023 Uiso 1 1 calc R U . . .
C34 C 0.2026(3) 0.2821(3) 0.15182(17) 0.0187(7) Uani 1 1 d . . . . .
H34A H 0.1437 0.3377 0.1287 0.022 Uiso 1 1 calc R U . . .
H34B H 0.3078 0.3177 0.1602 0.022 Uiso 1 1 calc R U . . .
C44 C 0.9358(3) 0.2335(3) 0.45172(18) 0.0210(7) Uani 1 1 d . . . . .
C27 C 0.6891(3) 0.4829(3) 0.06239(17) 0.0221(7) Uani 1 1 d . . . . .
H27 H 0.6110 0.4280 0.0236 0.027 Uiso 1 1 calc R U . . .
C47 C 0.6712(3) 0.1198(3) 0.25988(18) 0.0214(7) Uani 1 1 d . . . . .
H47A H 0.7186 0.0539 0.2564 0.032 Uiso 1 1 calc R U . . .
H47B H 0.6732 0.1631 0.2159 0.032 Uiso 1 1 calc R U . . .
H47C H 0.5691 0.0918 0.2609 0.032 Uiso 1 1 calc R U . . .
C49 C 0.7401(3) 0.4868(3) 0.43053(17) 0.0225(7) Uani 1 1 d . . . . .
H49A H 0.7609 0.5402 0.3937 0.034 Uiso 1 1 calc R U . . .
H49B H 0.7957 0.5211 0.4816 0.034 Uiso 1 1 calc R U . . .
H49C H 0.6348 0.4720 0.4274 0.034 Uiso 1 1 calc R U . . .
C33 C 0.2623(3) 0.1680(3) 0.26327(17) 0.0192(7) Uani 1 1 d . . . . .
H33A H 0.3682 0.2025 0.2737 0.023 Uiso 1 1 calc R U . . .
H33B H 0.2407 0.1487 0.3118 0.023 Uiso 1 1 calc R U . . .
C30 C 0.9971(4) 0.5995(3) 0.12275(19) 0.0265(8) Uani 1 1 d . . . . .
H30A H 1.0411 0.5670 0.0850 0.032 Uiso 1 1 calc R U . . .
H30B H 1.0762 0.6533 0.1606 0.032 Uiso 1 1 calc R U . . .
C39 C 0.2252(3) 0.0575(3) 0.20823(18) 0.0229(7) Uani 1 1 d . . . . .
H39 H 0.2857 0.0015 0.2309 0.028 Uiso 1 1 calc R U . . .
C29 C 0.9269(3) 0.5026(3) 0.16155(17) 0.0223(7) Uani 1 1 d . . . . .
H29 H 1.0033 0.4604 0.1874 0.027 Uiso 1 1 calc R U . . .
C38 C 0.0618(3) 0.0023(3) 0.19305(18) 0.0248(7) Uani 1 1 d . . . . .
H38A H 0.0381 -0.0687 0.1576 0.030 Uiso 1 1 calc R U . . .
H38B H 0.0391 -0.0192 0.2410 0.030 Uiso 1 1 calc R U . . .
C26 C 0.7600(4) 0.5812(3) 0.02398(18) 0.0270(8) Uani 1 1 d . . . . .
H26A H 0.6846 0.6230 -0.0019 0.032 Uiso 1 1 calc R U . . .
H26B H 0.8027 0.5492 -0.0145 0.032 Uiso 1 1 calc R U . . .
C36 C 0.0015(3) 0.1187(3) 0.08403(17) 0.0240(7) Uani 1 1 d . . . . .
H36A H -0.0580 0.1746 0.0619 0.029 Uiso 1 1 calc R U . . .
H36B H -0.0251 0.0483 0.0478 0.029 Uiso 1 1 calc R U . . .
C40 C 0.2579(4) 0.0870(3) 0.13393(19) 0.0260(8) Uani 1 1 d . . . . .
H40A H 0.2360 0.0157 0.0990 0.031 Uiso 1 1 calc R U . . .
H40B H 0.3634 0.1221 0.1429 0.031 Uiso 1 1 calc R U . . .
C24 C 0.8129(3) 0.7139(3) 0.14193(18) 0.0221(7) Uani 1 1 d . . . . .
H24A H 0.7386 0.7571 0.1166 0.027 Uiso 1 1 calc R U . . .
H24B H 0.8903 0.7686 0.1801 0.027 Uiso 1 1 calc R U . . .
C28 C 0.8060(4) 0.4186(3) 0.10288(18) 0.0243(7) Uani 1 1 d . . . . .
H28A H 0.7603 0.3556 0.1282 0.029 Uiso 1 1 calc R U . . .
H28B H 0.8489 0.3839 0.0655 0.029 Uiso 1 1 calc R U . . .
C48 C 1.0591(4) 0.1977(3) 0.50731(19) 0.0294(8) Uani 1 1 d . . . . .
H48A H 1.0399 0.1133 0.5060 0.044 Uiso 1 1 calc R U . . .
H48B H 1.0664 0.2318 0.5583 0.044 Uiso 1 1 calc R U . . .
H48C H 1.1515 0.2246 0.4939 0.044 Uiso 1 1 calc R U . . .
C25 C 0.8806(4) 0.6644(3) 0.08349(18) 0.0252(7) Uani 1 1 d . . . . .
H25 H 0.9269 0.7287 0.0584 0.030 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0145(2) 0.0146(2) 0.0165(2) 0.00075(16) 0.00208(16) 0.00488(16)
F5 0.0242(10) 0.0319(11) 0.0214(10) 0.0019(8) -0.0013(8) 0.0135(8)
F3 0.0360(11) 0.0184(10) 0.0269(10) -0.0040(8) 0.0142(8) 0.0074(8)
F1 0.0328(10) 0.0288(11) 0.0152(10) -0.0004(8) -0.0042(8) 0.0134(9)
F4 0.0275(10) 0.0336(11) 0.0132(9) -0.0025(8) 0.0006(8) 0.0021(8)
F2 0.0349(11) 0.0276(11) 0.0292(11) 0.0058(8) 0.0049(9) 0.0201(9)
N1 0.0138(12) 0.0199(14) 0.0180(14) -0.0005(11) 0.0020(10) 0.0048(11)
N2 0.0154(12) 0.0153(13) 0.0082(12) 0.0028(10) -0.0013(10) 0.0048(10)
N3 0.0136(12) 0.0143(13) 0.0231(14) 0.0031(11) 0.0073(11) 0.0014(10)
C2 0.0171(15) 0.0158(16) 0.0155(16) 0.0006(12) 0.0019(12) 0.0055(13)
C1 0.0177(15) 0.0161(16) 0.0132(15) 0.0031(12) -0.0007(12) 0.0059(13)
C11 0.0156(15) 0.0159(16) 0.0162(16) -0.0009(12) 0.0045(12) 0.0024(12)
C5 0.0142(14) 0.0164(16) 0.0159(16) 0.0025(12) 0.0006(12) 0.0051(12)
C6 0.0187(15) 0.0165(16) 0.0128(15) 0.0007(12) 0.0020(12) 0.0064(13)
C9 0.0170(15) 0.0180(16) 0.0120(15) 0.0049(12) 0.0017(12) 0.0035(13)
C43 0.0200(16) 0.0154(16) 0.0237(17) 0.0071(13) 0.0092(13) 0.0071(13)
C7 0.0234(16) 0.0186(17) 0.0130(15) 0.0027(12) 0.0060(13) 0.0065(13)
C3 0.0224(16) 0.0155(16) 0.0224(17) -0.0025(13) 0.0040(14) 0.0028(13)
C16 0.0141(15) 0.0206(17) 0.0179(17) 0.0034(13) 0.0028(13) 0.0051(13)
C15 0.0205(16) 0.0186(16) 0.0117(16) -0.0015(12) 0.0037(13) -0.0016(13)
C22 0.0164(15) 0.0209(17) 0.0164(16) 0.0018(13) 0.0003(13) 0.0050(13)
C4 0.0213(16) 0.0151(16) 0.0245(18) 0.0014(13) 0.0080(14) 0.0016(13)
C31 0.0147(15) 0.0187(16) 0.0128(15) -0.0002(12) 0.0003(12) 0.0039(13)
C41 0.0144(15) 0.0193(16) 0.0195(16) 0.0073(13) 0.0075(13) 0.0062(13)
C42 0.0172(15) 0.0163(16) 0.0191(16) 0.0035(13) 0.0079(13) 0.0015(13)
C37 0.0169(16) 0.0234(18) 0.0249(18) -0.0032(14) 0.0051(13) -0.0023(13)
C46 0.0162(15) 0.0229(17) 0.0152(16) 0.0046(13) 0.0066(12) 0.0055(13)
C14 0.0226(16) 0.0137(16) 0.0246(18) -0.0027(13) 0.0096(14) 0.0015(13)
C45 0.0188(15) 0.0262(18) 0.0145(16) 0.0011(13) 0.0026(13) 0.0041(14)
C8 0.0192(15) 0.0200(17) 0.0162(16) 0.0016(13) 0.0049(13) 0.0012(13)
C12 0.0203(16) 0.0200(17) 0.0136(16) 0.0028(13) 0.0028(13) 0.0018(13)
C21 0.0166(15) 0.0176(16) 0.0131(15) 0.0013(12) 0.0002(12) 0.0040(13)
C13 0.0203(16) 0.0188(17) 0.0221(18) 0.0070(13) 0.0032(13) 0.0090(13)
C35 0.0262(17) 0.0241(18) 0.0147(16) 0.0001(13) 0.0046(13) 0.0048(14)
C32 0.0181(15) 0.0238(17) 0.0158(16) -0.0002(13) 0.0032(13) 0.0032(13)
C23 0.0164(15) 0.0233(17) 0.0154(16) 0.0019(13) 0.0008(13) 0.0052(13)
C34 0.0226(16) 0.0183(17) 0.0175(16) 0.0036(13) 0.0074(13) 0.0066(13)
C44 0.0172(15) 0.0282(18) 0.0215(17) 0.0103(14) 0.0090(13) 0.0072(14)
C27 0.0212(16) 0.0309(19) 0.0115(16) -0.0008(13) -0.0013(13) 0.0070(14)
C47 0.0204(16) 0.0143(16) 0.0301(18) 0.0004(13) 0.0057(14) 0.0067(13)
C49 0.0263(17) 0.0245(18) 0.0160(16) -0.0012(13) 0.0016(13) 0.0101(14)
C33 0.0211(16) 0.0156(16) 0.0177(16) 0.0047(13) 0.0000(13) 0.0019(13)
C30 0.0244(17) 0.033(2) 0.0234(18) -0.0004(15) 0.0087(14) 0.0070(15)
C39 0.0249(17) 0.0165(17) 0.0245(18) 0.0026(13) 0.0005(14) 0.0049(14)
C29 0.0188(16) 0.0294(19) 0.0188(17) 0.0016(14) 0.0015(13) 0.0098(14)
C38 0.0312(18) 0.0164(17) 0.0230(18) 0.0018(14) 0.0048(15) -0.0013(14)
C26 0.0315(18) 0.036(2) 0.0163(17) 0.0056(15) 0.0078(14) 0.0103(16)
C36 0.0274(17) 0.0246(18) 0.0160(17) -0.0056(13) 0.0006(14) 0.0046(14)
C40 0.0247(17) 0.0198(17) 0.0310(19) -0.0066(14) 0.0052(15) 0.0040(14)
C24 0.0213(16) 0.0218(18) 0.0231(18) 0.0044(14) 0.0058(14) 0.0037(14)
C28 0.0320(18) 0.0252(18) 0.0205(17) 0.0002(14) 0.0118(15) 0.0115(15)
C48 0.0249(18) 0.034(2) 0.029(2) 0.0097(16) 0.0020(15) 0.0098(16)
C25 0.0272(17) 0.0292(19) 0.0214(18) 0.0069(14) 0.0105(14) 0.0042(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 1.696(2) . ?
Ni1 N2 1.905(2) . ?
Ni1 N1 1.913(3) . ?
F5 C16 1.342(3) . ?
F3 C14 1.333(3) . ?
F1 C12 1.345(3) . ?
F4 C15 1.343(3) . ?
F2 C13 1.348(3) . ?
N1 C5 1.351(4) . ?
N1 C2 1.402(4) . ?
N2 C9 1.344(4) . ?
N2 C6 1.400(4) . ?
N3 C41 1.348(4) . ?
C2 C1 1.397(4) . ?
C2 C3 1.410(4) . ?
C1 C6 1.391(4) . ?
C1 C11 1.493(4) . ?
C11 C16 1.389(4) . ?
C11 C12 1.393(4) . ?
C5 C4 1.414(4) . ?
C5 C21 1.508(4) . ?
C6 C7 1.414(4) . ?
C9 C8 1.425(4) . ?
C9 C31 1.506(4) . ?
C43 C42 1.381(4) . ?
C43 C44 1.395(4) . ?
C43 H43 0.9500 . ?
C7 C8 1.365(4) . ?
C7 H7 0.9500 . ?
C3 C4 1.366(4) . ?
C3 H3 0.9500 . ?
C16 C15 1.372(4) . ?
C15 C14 1.379(4) . ?
C22 C27 1.529(4) . ?
C22 C21 1.538(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C4 H4 0.9500 . ?
C31 C32 1.535(4) . ?
C31 C34 1.543(4) . ?
C31 C33 1.549(4) . ?
C41 C42 1.423(4) . ?
C41 C46 1.429(4) . ?
C42 C47 1.504(4) . ?
C37 C36 1.524(4) . ?
C37 C38 1.527(4) . ?
C37 C32 1.532(4) . ?
C37 H37 1.0000 . ?
C46 C45 1.397(4) . ?
C46 C49 1.492(4) . ?
C14 C13 1.377(4) . ?
C45 C44 1.393(4) . ?
C45 H45 0.9500 . ?
C8 H8 0.9500 . ?
C12 C13 1.367(4) . ?
C21 C23 1.537(4) . ?
C21 C24 1.547(4) . ?
C35 C40 1.525(4) . ?
C35 C34 1.528(4) . ?
C35 C36 1.530(4) . ?
C35 H35 1.0000 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C23 C29 1.544(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C44 C48 1.500(4) . ?
C27 C26 1.530(5) . ?
C27 C28 1.532(4) . ?
C27 H27 1.0000 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C33 C39 1.540(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C30 C29 1.520(5) . ?
C30 C25 1.528(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C39 C40 1.515(5) . ?
C39 C38 1.533(4) . ?
C39 H39 1.0000 . ?
C29 C28 1.529(4) . ?
C29 H29 1.0000 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C26 C25 1.532(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C24 C25 1.527(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C25 H25 1.0000 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N2 129.70(11) . . ?
N3 Ni1 N1 129.32(11) . . ?
N2 Ni1 N1 94.68(10) . . ?
C5 N1 C2 107.0(2) . . ?
C5 N1 Ni1 130.9(2) . . ?
C2 N1 Ni1 119.8(2) . . ?
C9 N2 C6 107.2(2) . . ?
C9 N2 Ni1 130.5(2) . . ?
C6 N2 Ni1 119.28(19) . . ?
C41 N3 Ni1 146.5(2) . . ?
C1 C2 N1 122.7(3) . . ?
C1 C2 C3 128.6(3) . . ?
N1 C2 C3 108.6(3) . . ?
C6 C1 C2 127.0(3) . . ?
C6 C1 C11 116.4(3) . . ?
C2 C1 C11 116.4(3) . . ?
C16 C11 C12 115.9(3) . . ?
C16 C11 C1 122.4(3) . . ?
C12 C11 C1 121.7(3) . . ?
N1 C5 C4 109.5(3) . . ?
N1 C5 C21 122.8(3) . . ?
C4 C5 C21 127.6(3) . . ?
C1 C6 N2 123.0(3) . . ?
C1 C6 C7 128.4(3) . . ?
N2 C6 C7 108.4(3) . . ?
N2 C9 C8 109.8(3) . . ?
N2 C9 C31 123.0(3) . . ?
C8 C9 C31 127.0(3) . . ?
C42 C43 C44 121.7(3) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C8 C7 C6 107.5(3) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C4 C3 C2 107.2(3) . . ?
C4 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
F5 C16 C15 118.4(3) . . ?
F5 C16 C11 119.2(3) . . ?
C15 C16 C11 122.5(3) . . ?
F4 C15 C16 120.6(3) . . ?
F4 C15 C14 119.5(3) . . ?
C16 C15 C14 119.9(3) . . ?
C27 C22 C21 110.9(2) . . ?
C27 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C27 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C3 C4 C5 107.7(3) . . ?
C3 C4 H4 126.1 . . ?
C5 C4 H4 126.1 . . ?
C9 C31 C32 110.5(2) . . ?
C9 C31 C34 110.2(2) . . ?
C32 C31 C34 108.5(2) . . ?
C9 C31 C33 111.1(2) . . ?
C32 C31 C33 107.7(2) . . ?
C34 C31 C33 108.8(2) . . ?
N3 C41 C42 120.2(3) . . ?
N3 C41 C46 120.5(3) . . ?
C42 C41 C46 119.2(3) . . ?
C43 C42 C41 119.8(3) . . ?
C43 C42 C47 120.8(3) . . ?
C41 C42 C47 119.5(3) . . ?
C36 C37 C38 109.8(3) . . ?
C36 C37 C32 109.2(3) . . ?
C38 C37 C32 109.8(3) . . ?
C36 C37 H37 109.3 . . ?
C38 C37 H37 109.3 . . ?
C32 C37 H37 109.3 . . ?
C45 C46 C41 118.2(3) . . ?
C45 C46 C49 121.2(3) . . ?
C41 C46 C49 120.6(3) . . ?
F3 C14 C13 120.3(3) . . ?
F3 C14 C15 120.5(3) . . ?
C13 C14 C15 119.2(3) . . ?
C44 C45 C46 122.4(3) . . ?
C44 C45 H45 118.8 . . ?
C46 C45 H45 118.8 . . ?
C7 C8 C9 107.1(3) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
F1 C12 C13 118.3(3) . . ?
F1 C12 C11 119.2(3) . . ?
C13 C12 C11 122.5(3) . . ?
C5 C21 C23 111.3(2) . . ?
C5 C21 C22 110.7(2) . . ?
C23 C21 C22 109.1(2) . . ?
C5 C21 C24 110.0(2) . . ?
C23 C21 C24 107.6(2) . . ?
C22 C21 C24 108.2(2) . . ?
F2 C13 C12 121.2(3) . . ?
F2 C13 C14 118.7(3) . . ?
C12 C13 C14 120.1(3) . . ?
C40 C35 C34 109.1(2) . . ?
C40 C35 C36 110.4(3) . . ?
C34 C35 C36 109.1(3) . . ?
C40 C35 H35 109.4 . . ?
C34 C35 H35 109.4 . . ?
C36 C35 H35 109.4 . . ?
C37 C32 C31 110.9(2) . . ?
C37 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C37 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
C21 C23 C29 110.1(2) . . ?
C21 C23 H23A 109.6 . . ?
C29 C23 H23A 109.6 . . ?
C21 C23 H23B 109.6 . . ?
C29 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C35 C34 C31 110.5(2) . . ?
C35 C34 H34A 109.6 . . ?
C31 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C31 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C45 C44 C43 118.5(3) . . ?
C45 C44 C48 120.8(3) . . ?
C43 C44 C48 120.7(3) . . ?
C22 C27 C26 109.5(3) . . ?
C22 C27 C28 108.6(2) . . ?
C26 C27 C28 109.8(3) . . ?
C22 C27 H27 109.6 . . ?
C26 C27 H27 109.6 . . ?
C28 C27 H27 109.6 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C39 C33 C31 109.8(2) . . ?
C39 C33 H33A 109.7 . . ?
C31 C33 H33A 109.7 . . ?
C39 C33 H33B 109.7 . . ?
C31 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C29 C30 C25 109.5(3) . . ?
C29 C30 H30A 109.8 . . ?
C25 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
C25 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
C40 C39 C38 108.8(3) . . ?
C40 C39 C33 109.7(3) . . ?
C38 C39 C33 109.9(3) . . ?
C40 C39 H39 109.4 . . ?
C38 C39 H39 109.4 . . ?
C33 C39 H39 109.4 . . ?
C30 C29 C28 109.8(3) . . ?
C30 C29 C23 109.9(3) . . ?
C28 C29 C23 108.9(2) . . ?
C30 C29 H29 109.4 . . ?
C28 C29 H29 109.4 . . ?
C23 C29 H29 109.4 . . ?
C37 C38 C39 109.3(2) . . ?
C37 C38 H38A 109.8 . . ?
C39 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
C39 C38 H38B 109.8 . . ?
H38A C38 H38B 108.3 . . ?
C27 C26 C25 109.5(3) . . ?
C27 C26 H26A 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
C37 C36 C35 109.0(2) . . ?
C37 C36 H36A 109.9 . . ?
C35 C36 H36A 109.9 . . ?
C37 C36 H36B 109.9 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
C39 C40 C35 110.1(3) . . ?
C39 C40 H40A 109.6 . . ?
C35 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
C35 C40 H40B 109.6 . . ?
H40A C40 H40B 108.2 . . ?
C25 C24 C21 111.1(3) . . ?
C25 C24 H24A 109.4 . . ?
C21 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C21 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C29 C28 C27 109.8(3) . . ?
C29 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
C29 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C24 C25 C30 109.5(3) . . ?
C24 C25 C26 109.2(3) . . ?
C30 C25 C26 109.5(3) . . ?
C24 C25 H25 109.6 . . ?
C30 C25 H25 109.6 . . ?
C26 C25 H25 109.6 . . ?
_refine_diff_density_max 0.815
_refine_diff_density_min -0.637
_refine_diff_density_rms 0.089
_shelx_res_file
;
dyy_10.res created by SHELXL-2014/7
TITL DYY_10_a.res in P-1
REM Old TITL DYY_10 in P-1
REM SHELXT solution in P-1
REM R1 0.160, Rweak 0.013, Alpha 0.044, Orientation as input
REM Formula found by SHELXT: C55 Ni
CELL 0.71073 9.5949 11.8426 18.3253 92.953 104.293 100.626
ZERR 2 0.0007 0.001 0.0014 0.003 0.002 0.002
LATT 1
SFAC C H F N Ni
UNIT 88 90 10 6 2
L.S. 50
PLAN 20
SIZE 0.03 0.2 0.26
TEMP -173.12
BOND $H
LIST 4
ABIN
fmap 2
acta
OMIT 0 1 1
REM
REM
REM
WGHT 0.086600 0.842000
FVAR 0.13619
NI1 5 0.508711 0.442449 0.267046 11.00000 0.01449 0.01457 =
0.01655 0.00075 0.00208 0.00488
F5 3 0.556612 0.708032 0.501614 11.00000 0.02420 0.03192 =
0.02144 0.00194 -0.00133 0.01346
F3 3 0.303024 1.003486 0.528469 11.00000 0.03605 0.01841 =
0.02687 -0.00396 0.01422 0.00738
F1 3 0.195862 0.784188 0.294445 11.00000 0.03277 0.02880 =
0.01519 -0.00041 -0.00419 0.01336
F4 3 0.508672 0.880149 0.588098 11.00000 0.02750 0.03362 =
0.01318 -0.00247 0.00061 0.00206
F2 3 0.144624 0.953194 0.382913 11.00000 0.03487 0.02755 =
0.02925 0.00575 0.00492 0.02010
N1 4 0.565538 0.605491 0.264786 11.00000 0.01378 0.01987 =
0.01796 -0.00049 0.00195 0.00483
N2 4 0.323738 0.449452 0.285863 11.00000 0.01541 0.01532 =
0.00817 0.00284 -0.00127 0.00478
N3 4 0.615551 0.343503 0.289349 11.00000 0.01363 0.01429 =
0.02310 0.00310 0.00729 0.00136
C2 1 0.525430 0.681661 0.313235 11.00000 0.01712 0.01584 =
0.01547 0.00060 0.00192 0.00554
C1 1 0.408727 0.648741 0.345662 11.00000 0.01772 0.01609 =
0.01321 0.00307 -0.00071 0.00592
C11 1 0.378092 0.740154 0.395161 11.00000 0.01556 0.01592 =
0.01619 -0.00091 0.00447 0.00242
C5 1 0.671850 0.667959 0.238360 11.00000 0.01417 0.01640 =
0.01588 0.00250 0.00057 0.00513
C6 1 0.312850 0.542029 0.333428 11.00000 0.01868 0.01649 =
0.01280 0.00072 0.00196 0.00644
C9 1 0.205413 0.365442 0.280491 11.00000 0.01695 0.01800 =
0.01203 0.00494 0.00170 0.00350
C43 1 0.860896 0.163557 0.384812 11.00000 0.01995 0.01543 =
0.02367 0.00712 0.00924 0.00714
AFIX 43
H43 2 0.885453 0.090851 0.375962 11.00000 -1.20000
AFIX 0
C7 1 0.185047 0.509689 0.359050 11.00000 0.02340 0.01862 =
0.01302 0.00271 0.00602 0.00655
AFIX 43
H7 2 0.152194 0.555366 0.392936 11.00000 -1.20000
AFIX 0
C3 1 0.613241 0.792337 0.316879 11.00000 0.02244 0.01553 =
0.02237 -0.00251 0.00397 0.00283
AFIX 43
H3 2 0.610555 0.859985 0.346267 11.00000 -1.20000
AFIX 0
C16 1 0.454407 0.767677 0.470843 11.00000 0.01405 0.02058 =
0.01785 0.00343 0.00278 0.00505
C15 1 0.429676 0.854223 0.515748 11.00000 0.02052 0.01859 =
0.01172 -0.00152 0.00367 -0.00158
C22 1 0.621604 0.532555 0.120964 11.00000 0.01638 0.02086 =
0.01640 0.00177 0.00027 0.00500
AFIX 23
H22A 2 0.574505 0.468821 0.145249 11.00000 -1.20000
H22B 2 0.544864 0.573412 0.095404 11.00000 -1.20000
AFIX 0
C4 1 0.702865 0.784052 0.270247 11.00000 0.02134 0.01508 =
0.02454 0.00141 0.00797 0.00157
AFIX 43
H4 2 0.773411 0.845290 0.260897 11.00000 -1.20000
AFIX 0
C31 1 0.170310 0.255770 0.228304 11.00000 0.01470 0.01875 =
0.01279 -0.00019 0.00032 0.00387
C41 1 0.714061 0.306017 0.343631 11.00000 0.01438 0.01931 =
0.01949 0.00731 0.00752 0.00622
C42 1 0.751949 0.197325 0.331120 11.00000 0.01720 0.01626 =
0.01911 0.00349 0.00786 0.00149
C37 1 -0.030287 0.088259 0.158906 11.00000 0.01694 0.02338 =
0.02493 -0.00324 0.00512 -0.00230
AFIX 13
H37 2 -0.136875 0.052917 0.149897 11.00000 -1.20000
AFIX 0
C46 1 0.784139 0.375918 0.413637 11.00000 0.01625 0.02288 =
0.01515 0.00459 0.00658 0.00551
C14 1 0.325492 0.917232 0.485988 11.00000 0.02259 0.01367 =
0.02456 -0.00266 0.00964 0.00155
C45 1 0.895143 0.338029 0.465163 11.00000 0.01876 0.02617 =
0.01451 0.00115 0.00262 0.00409
AFIX 43
H45 2 0.944715 0.385284 0.511055 11.00000 -1.20000
AFIX 0
C8 1 0.117542 0.400849 0.326188 11.00000 0.01925 0.02003 =
0.01622 0.00162 0.00490 0.00125
AFIX 43
H8 2 0.028707 0.356964 0.332576 11.00000 -1.20000
AFIX 0
C12 1 0.273227 0.805279 0.367415 11.00000 0.02030 0.01998 =
0.01358 0.00275 0.00276 0.00184
C21 1 0.739491 0.616874 0.181803 11.00000 0.01661 0.01760 =
0.01314 0.00126 0.00021 0.00400
C13 1 0.246654 0.891449 0.411367 11.00000 0.02030 0.01883 =
0.02212 0.00695 0.00320 0.00895
C35 1 0.165033 0.171323 0.098172 11.00000 0.02622 0.02415 =
0.01468 0.00009 0.00461 0.00477
AFIX 13
H35 2 0.187074 0.189841 0.049061 11.00000 -1.20000
AFIX 0
C32 1 0.007429 0.198418 0.213479 11.00000 0.01809 0.02379 =
0.01581 -0.00022 0.00319 0.00316
AFIX 23
H32A 2 -0.014479 0.179179 0.261939 11.00000 -1.20000
H32B 2 -0.054189 0.253107 0.191653 11.00000 -1.20000
AFIX 0
C23 1 0.858723 0.552944 0.220649 11.00000 0.01642 0.02333 =
0.01539 0.00185 0.00080 0.00518
AFIX 23
H23A 2 0.815143 0.489761 0.246589 11.00000 -1.20000
H23B 2 0.936224 0.607015 0.259179 11.00000 -1.20000
AFIX 0
C34 1 0.202577 0.282093 0.151822 11.00000 0.02263 0.01834 =
0.01748 0.00362 0.00740 0.00658
AFIX 23
H34A 2 0.143737 0.337706 0.128673 11.00000 -1.20000
H34B 2 0.307772 0.317749 0.160236 11.00000 -1.20000
AFIX 0
C44 1 0.935808 0.233507 0.451720 11.00000 0.01719 0.02822 =
0.02150 0.01029 0.00899 0.00722
C27 1 0.689136 0.482866 0.062391 11.00000 0.02120 0.03093 =
0.01148 -0.00078 -0.00134 0.00696
AFIX 13
H27 2 0.610951 0.428041 0.023553 11.00000 -1.20000
AFIX 0
C47 1 0.671178 0.119801 0.259880 11.00000 0.02038 0.01435 =
0.03013 0.00040 0.00571 0.00673
AFIX 137
H47A 2 0.718645 0.053924 0.256396 11.00000 -1.50000
H47B 2 0.673197 0.163135 0.215885 11.00000 -1.50000
H47C 2 0.569067 0.091833 0.260943 11.00000 -1.50000
AFIX 0
C49 1 0.740101 0.486844 0.430529 11.00000 0.02633 0.02453 =
0.01597 -0.00118 0.00159 0.01005
AFIX 137
H49A 2 0.760940 0.540227 0.393654 11.00000 -1.50000
H49B 2 0.795676 0.521134 0.481624 11.00000 -1.50000
H49C 2 0.634771 0.472008 0.427400 11.00000 -1.50000
AFIX 0
C33 1 0.262281 0.167984 0.263272 11.00000 0.02114 0.01559 =
0.01771 0.00474 0.00003 0.00193
AFIX 23
H33A 2 0.368235 0.202533 0.273686 11.00000 -1.20000
H33B 2 0.240694 0.148658 0.311787 11.00000 -1.20000
AFIX 0
C30 1 0.997088 0.599454 0.122755 11.00000 0.02435 0.03312 =
0.02337 -0.00040 0.00866 0.00699
AFIX 23
H30A 2 1.041072 0.566991 0.085038 11.00000 -1.20000
H30B 2 1.076207 0.653252 0.160645 11.00000 -1.20000
AFIX 0
C39 1 0.225150 0.057474 0.208227 11.00000 0.02489 0.01650 =
0.02445 0.00260 0.00046 0.00485
AFIX 13
H39 2 0.285733 0.001545 0.230872 11.00000 -1.20000
AFIX 0
C29 1 0.926866 0.502593 0.161548 11.00000 0.01879 0.02935 =
0.01878 0.00161 0.00147 0.00980
AFIX 13
H29 2 1.003311 0.460378 0.187363 11.00000 -1.20000
AFIX 0
C38 1 0.061811 0.002314 0.193047 11.00000 0.03119 0.01641 =
0.02296 0.00183 0.00479 -0.00133
AFIX 23
H38A 2 0.038149 -0.068658 0.157619 11.00000 -1.20000
H38B 2 0.039091 -0.019187 0.240953 11.00000 -1.20000
AFIX 0
C26 1 0.759982 0.581155 0.023982 11.00000 0.03154 0.03566 =
0.01629 0.00559 0.00776 0.01025
AFIX 23
H26A 2 0.684631 0.623011 -0.001872 11.00000 -1.20000
H26B 2 0.802691 0.549239 -0.014488 11.00000 -1.20000
AFIX 0
C36 1 0.001452 0.118666 0.084032 11.00000 0.02744 0.02459 =
0.01600 -0.00563 0.00060 0.00456
AFIX 23
H36A 2 -0.057951 0.174572 0.061927 11.00000 -1.20000
H36B 2 -0.025104 0.048320 0.047843 11.00000 -1.20000
AFIX 0
C40 1 0.257873 0.087041 0.133927 11.00000 0.02470 0.01984 =
0.03102 -0.00665 0.00516 0.00396
AFIX 23
H40A 2 0.236016 0.015709 0.098992 11.00000 -1.20000
H40B 2 0.363377 0.122121 0.142892 11.00000 -1.20000
AFIX 0
C24 1 0.812887 0.713930 0.141928 11.00000 0.02134 0.02185 =
0.02309 0.00436 0.00577 0.00369
AFIX 23
H24A 2 0.738647 0.757097 0.116563 11.00000 -1.20000
H24B 2 0.890314 0.768584 0.180130 11.00000 -1.20000
AFIX 0
C28 1 0.805993 0.418625 0.102882 11.00000 0.03201 0.02517 =
0.02052 0.00022 0.01175 0.01150
AFIX 23
H28A 2 0.760287 0.355611 0.128208 11.00000 -1.20000
H28B 2 0.848886 0.383914 0.065503 11.00000 -1.20000
AFIX 0
C48 1 1.059106 0.197704 0.507307 11.00000 0.02490 0.03396 =
0.02894 0.00975 0.00196 0.00978
AFIX 137
H48A 2 1.039872 0.113333 0.506028 11.00000 -1.50000
H48B 2 1.066431 0.231810 0.558327 11.00000 -1.50000
H48C 2 1.151545 0.224587 0.493872 11.00000 -1.50000
AFIX 0
C25 1 0.880609 0.664410 0.083491 11.00000 0.02722 0.02917 =
0.02142 0.00686 0.01054 0.00417
AFIX 13
H25 2 0.926946 0.728661 0.058412 11.00000 -1.20000
AFIX 0
HKLF 4
REM DYY_10_a.res in P-1
REM R1 = 0.0517 for 5464 Fo > 4sig(Fo) and 0.0719 for all 6992 data
REM 481 parameters refined using 0 restraints
END
WGHT 0.0866 0.8420
REM Highest difference peak 0.815, deepest hole -0.637, 1-sigma level 0.089
Q1 1 0.4797 0.5208 0.2877 11.00000 0.05 0.81
Q2 1 0.5320 0.3655 0.2439 11.00000 0.05 0.78
Q3 1 0.3965 0.4292 0.2720 11.00000 0.05 0.71
Q4 1 0.5600 0.5298 0.2727 11.00000 0.05 0.66
Q5 1 0.6345 0.4536 0.2617 11.00000 0.05 0.59
Q6 1 0.4480 0.3608 0.2594 11.00000 0.05 0.57
Q7 1 0.6570 0.3816 0.2444 11.00000 0.05 0.47
Q8 1 0.3294 0.3713 0.2631 11.00000 0.05 0.45
Q9 1 0.3433 0.5153 0.2961 11.00000 0.05 0.44
Q10 1 0.7168 0.5196 0.2780 11.00000 0.05 0.41
Q11 1 0.5383 0.4618 0.2141 11.00000 0.05 0.40
Q12 1 0.2196 0.5458 0.3263 11.00000 0.05 0.38
Q13 1 0.5486 0.6256 0.2981 11.00000 0.05 0.37
Q14 1 0.3639 0.5923 0.3345 11.00000 0.05 0.36
Q15 1 0.2160 0.7978 0.3970 11.00000 0.05 0.36
Q16 1 0.4989 0.6570 0.3478 11.00000 0.05 0.35
Q17 1 0.5649 0.6314 0.4826 11.00000 0.05 0.35
Q18 1 0.5582 0.7475 0.3063 11.00000 0.05 0.35
Q19 1 0.1603 0.3615 0.3088 11.00000 0.05 0.34
Q20 1 0.4811 0.4227 0.3249 11.00000 0.05 0.33
;
_shelx_res_checksum 75212
_shelx_fab_file
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7 7 0 0.6075 0.0000
7 7 1 -0.3423 0.0000
7 7 2 -1.3266 0.0000
7 7 3 -1.3931 0.0000
7 7 4 -0.7568 0.0000
7 7 5 -0.3177 0.0000
7 8 0 1.4786 0.0000
7 8 1 1.2937 0.0000
7 8 2 0.2748 0.0000
7 8 3 -0.6815 0.0000
8 -11 0 2.6441 0.0000
8 -11 1 1.1251 0.0000
8 -11 2 -0.1071 0.0000
8 -11 3 -0.5310 0.0000
8 -10 0 4.4972 0.0000
8 -10 1 3.6132 0.0000
8 -10 2 1.9318 0.0000
8 -10 3 0.4545 0.0000
8 -10 4 -0.3038 0.0000
8 -10 5 -0.4502 0.0000
8 -9 0 3.4267 0.0000
8 -9 1 5.1807 0.0000
8 -9 2 5.3197 0.0000
8 -9 3 4.0812 0.0000
8 -9 4 2.3180 0.0000
8 -9 5 0.7817 0.0000
8 -9 6 -0.1443 0.0000
8 -9 7 -0.3971 0.0000
8 -8 0 -0.5362 0.0000
8 -8 1 1.9228 0.0000
8 -8 2 4.3521 0.0000
8 -8 3 5.8136 0.0000
8 -8 4 5.8701 0.0000
8 -8 5 4.6222 0.0000
8 -8 6 2.6678 0.0000
8 -8 7 0.8447 0.0000
8 -8 8 -0.2480 0.0000
8 -7 0 -2.1350 0.0000
8 -7 1 -1.4910 0.0000
8 -7 2 0.1102 0.0000
8 -7 3 2.2662 0.0000
8 -7 4 4.2931 0.0000
8 -7 5 5.3778 0.0000
8 -7 6 5.1252 0.0000
8 -7 7 3.8677 0.0000
8 -7 8 2.3102 0.0000
8 -7 9 0.9884 0.0000
8 -6 0 -0.4811 0.0000
8 -6 1 -1.3404 0.0000
8 -6 2 -1.3809 0.0000
8 -6 3 -0.3614 0.0000
8 -6 4 1.5532 0.0000
8 -6 5 3.4197 0.0000
8 -6 6 4.1872 0.0000
8 -6 7 3.7598 0.0000
8 -6 8 2.9603 0.0000
8 -6 9 2.4275 0.0000
8 -6 10 1.9945 0.0000
8 -5 0 2.5918 0.0000
8 -5 1 1.4334 0.0000
8 -5 2 0.0386 0.0000
8 -5 3 -1.0433 0.0000
8 -5 4 -0.8302 0.0000
8 -5 5 0.9522 0.0000
8 -5 6 3.1707 0.0000
8 -5 7 4.2728 0.0000
8 -5 8 3.8256 0.0000
8 -5 9 2.6690 0.0000
8 -5 10 1.7064 0.0000
8 -4 0 1.8304 0.0000
8 -4 1 1.3136 0.0000
8 -4 2 0.6830 0.0000
8 -4 3 -0.0758 0.0000
8 -4 4 -0.6148 0.0000
8 -4 5 -0.3593 0.0000
8 -4 6 0.7312 0.0000
8 -4 7 1.9120 0.0000
8 -4 8 2.4244 0.0000
8 -4 9 2.2665 0.0000
8 -4 10 1.9465 0.0000
8 -4 11 1.7014 0.0000
8 -3 0 0.6859 0.0000
8 -3 1 0.1547 0.0000
8 -3 2 -0.4301 0.0000
8 -3 3 -1.0882 0.0000
8 -3 4 -1.6778 0.0000
8 -3 5 -1.7807 0.0000
8 -3 6 -1.1295 0.0000
8 -3 7 -0.0920 0.0000
8 -3 8 0.5920 0.0000
8 -3 9 0.6492 0.0000
8 -3 10 0.5666 0.0000
8 -3 11 0.8672 0.0000
8 -2 0 0.0633 0.0000
8 -2 1 -0.7359 0.0000
8 -2 2 -1.2627 0.0000
8 -2 3 -1.4481 0.0000
8 -2 4 -1.5538 0.0000
8 -2 5 -1.7772 0.0000
8 -2 6 -1.8719 0.0000
8 -2 7 -1.3675 0.0000
8 -2 8 -0.2442 0.0000
8 -2 9 0.8483 0.0000
8 -2 10 1.2515 0.0000
8 -2 11 1.0016 0.0000
8 -1 0 0.5274 0.0000
8 -1 1 0.0365 0.0000
8 -1 2 -1.0568 0.0000
8 -1 3 -2.3761 0.0000
8 -1 4 -3.2150 0.0000
8 -1 5 -3.1125 0.0000
8 -1 6 -2.2729 0.0000
8 -1 7 -1.2203 0.0000
8 -1 8 -0.2326 0.0000
8 -1 9 0.6436 0.0000
8 -1 10 1.2396 0.0000
8 -1 11 1.3107 0.0000
8 0 0 -0.7895 0.0000
8 0 1 -0.2710 0.0000
8 0 2 -0.1409 0.0000
8 0 3 -0.7549 0.0000
8 0 4 -2.0593 0.0000
8 0 5 -3.3649 0.0000
8 0 6 -3.9167 0.0000
8 0 7 -3.5443 0.0000
8 0 8 -2.6248 0.0000
8 0 9 -1.6276 0.0000
8 0 10 -0.8591 0.0000
8 1 0 -1.6148 0.0000
8 1 1 -0.7844 0.0000
8 1 2 0.0026 0.0000
8 1 3 0.2102 0.0000
8 1 4 -0.4158 0.0000
8 1 5 -1.5538 0.0000
8 1 6 -2.6175 0.0000
8 1 7 -3.2547 0.0000
8 1 8 -3.4015 0.0000
8 1 9 -3.0703 0.0000
8 1 10 -2.3760 0.0000
8 2 0 -1.9765 0.0000
8 2 1 -2.1964 0.0000
8 2 2 -1.3680 0.0000
8 2 3 0.1276 0.0000
8 2 4 1.1826 0.0000
8 2 5 1.1132 0.0000
8 2 6 0.1750 0.0000
8 2 7 -0.9887 0.0000
8 2 8 -1.9239 0.0000
8 2 9 -2.3257 0.0000
8 3 0 -0.2222 0.0000
8 3 1 -1.0203 0.0000
8 3 2 -1.6675 0.0000
8 3 3 -1.4520 0.0000
8 3 4 -0.4947 0.0000
8 3 5 0.4902 0.0000
8 3 6 1.0054 0.0000
8 3 7 0.9947 0.0000
8 3 8 0.5485 0.0000
8 4 0 0.4937 0.0000
8 4 1 0.6425 0.0000
8 4 2 0.5004 0.0000
8 4 3 0.3288 0.0000
8 4 4 0.1453 0.0000
8 4 5 -0.2491 0.0000
8 4 6 -0.7442 0.0000
8 4 7 -0.9203 0.0000
8 5 0 1.3414 0.0000
8 5 1 1.9348 0.0000
8 5 2 1.5034 0.0000
8 5 3 0.6476 0.0000
8 5 4 0.0774 0.0000
8 5 5 -0.2155 0.0000
8 5 6 -0.5424 0.0000
8 6 0 0.0076 0.0000
8 6 1 0.5264 0.0000
8 6 2 0.6349 0.0000
8 6 3 0.1794 0.0000
8 6 4 -0.2051 0.0000
8 7 0 -0.5897 0.0000
8 7 1 -0.7923 0.0000
9 -10 0 -2.6391 0.0000
9 -10 1 -2.4923 0.0000
9 -9 0 -1.6412 0.0000
9 -9 1 -3.2701 0.0000
9 -9 2 -4.0316 0.0000
9 -9 3 -3.7260 0.0000
9 -9 4 -2.6442 0.0000
9 -8 0 0.6158 0.0000
9 -8 1 -0.4861 0.0000
9 -8 2 -1.8832 0.0000
9 -8 3 -3.2986 0.0000
9 -8 4 -4.1739 0.0000
9 -8 5 -3.9867 0.0000
9 -8 6 -2.8254 0.0000
9 -7 0 1.7462 0.0000
9 -7 1 1.1575 0.0000
9 -7 2 0.2726 0.0000
9 -7 3 -0.9261 0.0000
9 -7 4 -2.2022 0.0000
9 -7 5 -2.8883 0.0000
9 -7 6 -2.5656 0.0000
9 -7 7 -1.6056 0.0000
9 -6 0 0.2435 0.0000
9 -6 1 0.7726 0.0000
9 -6 2 1.0595 0.0000
9 -6 3 0.7702 0.0000
9 -6 4 -0.3746 0.0000
9 -6 5 -1.8034 0.0000
9 -6 6 -2.3726 0.0000
9 -6 7 -1.6436 0.0000
9 -5 0 -0.9180 0.0000
9 -5 1 -0.2249 0.0000
9 -5 2 0.6012 0.0000
9 -5 3 1.4424 0.0000
9 -5 4 1.6848 0.0000
9 -5 5 0.7501 0.0000
9 -5 6 -0.9923 0.0000
9 -5 7 -2.3296 0.0000
9 -5 8 -2.3922 0.0000
9 -4 0 0.8044 0.0000
9 -4 1 2.0108 0.0000
9 -4 2 2.7313 0.0000
9 -4 3 2.7713 0.0000
9 -4 4 2.3024 0.0000
9 -4 5 1.5101 0.0000
9 -4 6 0.5069 0.0000
9 -4 7 -0.4302 0.0000
9 -4 8 -0.8811 0.0000
9 -3 0 0.7802 0.0000
9 -3 1 1.9705 0.0000
9 -3 2 2.9184 0.0000
9 -3 3 3.3247 0.0000
9 -3 4 3.2546 0.0000
9 -3 5 2.9623 0.0000
9 -3 6 2.4841 0.0000
9 -3 7 1.6813 0.0000
9 -3 8 0.7086 0.0000
9 -2 0 0.2867 0.0000
9 -2 1 1.3072 0.0000
9 -2 2 2.5393 0.0000
9 -2 3 3.3199 0.0000
9 -2 4 3.2067 0.0000
9 -2 5 2.5773 0.0000
9 -2 6 2.1689 0.0000
9 -2 7 2.0637 0.0000
9 -2 8 1.6528 0.0000
9 -1 0 -0.1018 0.0000
9 -1 1 -0.4326 0.0000
9 -1 2 0.0721 0.0000
9 -1 3 1.5386 0.0000
9 -1 4 3.0476 0.0000
9 -1 5 3.4617 0.0000
9 -1 6 2.6856 0.0000
9 -1 7 1.5977 0.0000
9 -1 8 0.8755 0.0000
9 0 0 0.6217 0.0000
9 0 1 -0.0279 0.0000
9 0 2 -0.5391 0.0000
9 0 3 -0.4408 0.0000
9 0 4 0.3569 0.0000
9 0 5 1.2476 0.0000
9 0 6 1.5865 0.0000
9 0 7 1.3745 0.0000
9 1 0 1.6065 0.0000
9 1 1 1.1021 0.0000
9 1 2 0.0628 0.0000
9 1 3 -0.8118 0.0000
9 1 4 -0.8151 0.0000
9 1 5 -0.0878 0.0000
9 1 6 0.6248 0.0000
9 1 7 0.8941 0.0000
9 2 0 1.0872 0.0000
9 2 1 2.0908 0.0000
9 2 2 2.2293 0.0000
9 2 3 1.1013 0.0000
9 2 4 -0.3763 0.0000
9 2 5 -1.0563 0.0000
9 2 6 -0.7524 0.0000
9 3 0 -0.3514 0.0000
9 3 1 -0.3118 0.0000
9 3 2 0.1530 0.0000
9 3 3 0.5089 0.0000
9 3 4 0.4231 0.0000
9 3 5 0.0894 0.0000
9 4 0 -0.2782 0.0000
9 4 1 -0.5440 0.0000
9 4 2 -0.8598 0.0000
9 4 3 -1.2114 0.0000
9 4 4 -1.4149 0.0000
9 5 0 -0.6571 0.0000
9 5 1 -0.8503 0.0000
9 5 2 -0.5904 0.0000
10 -8 0 -0.0876 0.0000
10 -8 1 0.0915 0.0000
10 -7 0 -1.3875 0.0000
10 -7 1 -0.7632 0.0000
10 -7 2 -0.2730 0.0000
10 -7 3 0.1087 0.0000
10 -6 0 -0.1294 0.0000
10 -6 1 -0.4958 0.0000
10 -6 2 -0.8664 0.0000
10 -6 3 -1.1059 0.0000
10 -6 4 -0.9184 0.0000
10 -5 0 -0.7634 0.0000
10 -5 1 -1.4163 0.0000
10 -5 2 -1.7386 0.0000
10 -5 3 -1.6706 0.0000
10 -5 4 -1.4704 0.0000
10 -5 5 -1.2233 0.0000
10 -4 0 -2.1064 0.0000
10 -4 1 -3.1315 0.0000
10 -4 2 -3.8076 0.0000
10 -4 3 -3.4883 0.0000
10 -4 4 -2.2578 0.0000
10 -4 5 -0.9342 0.0000
10 -3 0 -2.5059 0.0000
10 -3 1 -2.7968 0.0000
10 -3 2 -3.0271 0.0000
10 -3 3 -2.8956 0.0000
10 -3 4 -2.2102 0.0000
10 -3 5 -1.4185 0.0000
10 -2 0 -1.3196 0.0000
10 -2 1 -1.4126 0.0000
10 -2 2 -1.8882 0.0000
10 -2 3 -2.6165 0.0000
10 -2 4 -2.7592 0.0000
10 -2 5 -1.9681 0.0000
10 -1 0 -0.4332 0.0000
10 -1 1 0.0532 0.0000
10 -1 2 0.4657 0.0000
10 -1 3 0.1140 0.0000
10 -1 4 -0.8860 0.0000
10 -1 5 -1.5525 0.0000
10 0 0 -0.2036 0.0000
10 0 1 0.0276 0.0000
10 0 2 0.3447 0.0000
10 0 3 0.5449 0.0000
10 0 4 0.3985 0.0000
10 1 0 -0.8604 0.0000
10 1 1 -1.0654 0.0000
10 1 2 -0.5062 0.0000
10 1 3 0.4944 0.0000
10 2 0 0.2418 0.0000
10 2 1 -0.3964 0.0000
10 2 2 -1.0119 0.0000
10 3 0 -0.4153 0.0000
11 -4 0 1.5351 0.0000
11 -3 0 2.1814 0.0000
11 -2 0 0.9229 0.0000
0 0 0 0.0 0.0
_shelx_fab_checksum 1579
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_LNiNAd
_database_code_depnum_ccdc_archive 'CCDC 1953732'
loop_
_audit_author_name
_audit_author_address
'Shao-Liang Zheng'
;Harvard Univerisity
United States of America
;
_audit_update_record
;
2019-09-16 deposited with the CCDC. 2019-12-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C45 H49 F5 N3 Ni'
_chemical_formula_weight 785.58
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_H-M_alt 'P n a 21'
_space_group_name_Hall 'P 2c -2n'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 14.1294(9)
_cell_length_b 16.6197(8)
_cell_length_c 15.8282(8)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3716.9(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9905
_cell_measurement_theta_min 2.791
_cell_measurement_theta_max 66.626
_exptl_crystal_description needle
_exptl_crystal_colour pink
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.404
_exptl_crystal_F_000 1652
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.120
_exptl_crystal_size_mid 0.080
_exptl_crystal_size_min 0.020
_exptl_absorpt_coefficient_mu 1.275
_shelx_estimated_absorpt_T_min 0.862
_shelx_estimated_absorpt_T_max 0.975
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5528
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details SADBAS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source 'I/mS microfocus tube'
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 41286
_diffrn_reflns_av_unetI/netI 0.0866
_diffrn_reflns_av_R_equivalents 0.1104
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 3.856
_diffrn_reflns_theta_max 67.214
_diffrn_reflns_theta_full 67.214
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total 6222
_reflns_number_gt 3085
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.930
_reflns_Friedel_fraction_max 0.975
_reflns_Friedel_fraction_full 0.975
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_cell_refinement 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_reduction 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)'
_refine_special_details
;
Refined as a 2-component inversion twin. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. All on-H atoms, including the disorder fragments were located in difference-Fourier maps, and then refined anisotropically. The restraints on bond lengths and constrants of the atomic displacement parameters on each pair of disorder fragments (SADI/SAME and EADP instructions of SHELXL-2014), as well as the restraints of the atomic displacement parameters (SIMU/DELU/RIGU instructions of SHELXL-2014) if necessary, have been applied for the disorder refinement.
;
# start Validation Reply Form
_vrf_PLAT090_LNiNAd
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.31 Note
RESPONSE: The structure is refined with restraints and constraints due to disorder.
;
# end Validation Reply Form
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+12.3867P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.35(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns 6222
_refine_ls_number_parameters 631
_refine_ls_number_restraints 1015
_refine_ls_R_factor_all 0.1623
_refine_ls_R_factor_gt 0.0792
_refine_ls_wR_factor_ref 0.2265
_refine_ls_wR_factor_gt 0.1800
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 0.985
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.61322(12) -0.73058(8) -0.5257(4) 0.0464(5) Uani 1 1 d D U . . .
C1 C -0.559(4) -0.539(3) -0.5247(18) 0.037(8) Uani 0.384(8) 1 d D U P A 1
N1 N -0.638(3) -0.6449(19) -0.603(2) 0.047(7) Uani 0.384(8) 1 d D U P A 1
C2 C -0.591(3) -0.570(2) -0.600(2) 0.045(7) Uani 0.384(8) 1 d D U P A 1
C3 C -0.609(4) -0.532(3) -0.678(3) 0.065(7) Uani 0.384(8) 1 d D U P A 1
H3 H -0.5820 -0.4828 -0.6962 0.079 Uiso 0.384(8) 1 calc R U P A 1
C4 C -0.669(3) -0.577(2) -0.724(2) 0.061(6) Uani 0.384(8) 1 d D U P A 1
H4 H -0.6980 -0.5623 -0.7759 0.073 Uiso 0.384(8) 1 calc R U P A 1
C5 C -0.681(3) -0.649(2) -0.678(2) 0.049(5) Uani 0.384(8) 1 d D U P A 1
N2 N -0.612(4) -0.6572(19) -0.4344(19) 0.034(7) Uani 0.384(8) 1 d D U P A 1
C6 C -0.5770(12) -0.5788(11) -0.4498(10) 0.046(4) Uani 0.384(8) 1 d D U P A 1
C7 C -0.551(3) -0.548(3) -0.367(2) 0.048(7) Uani 0.384(8) 1 d D U P A 1
H7 H -0.5076 -0.5052 -0.3554 0.058 Uiso 0.384(8) 1 calc R U P A 1
C8 C -0.604(3) -0.594(3) -0.308(2) 0.055(8) Uani 0.384(8) 1 d D U P A 1
H8 H -0.6181 -0.5799 -0.2510 0.067 Uiso 0.384(8) 1 calc R U P A 1
C9 C -0.631(3) -0.666(3) -0.349(2) 0.044(5) Uani 0.384(8) 1 d D U P A 1
C11 C -0.5003(19) -0.4657(5) -0.533(5) 0.048(3) Uani 0.384(8) 1 d G U P A 1
C12 C -0.5517(10) -0.3947(8) -0.540(4) 0.044(6) Uani 0.384(8) 1 d DG U P A 1
C13 C -0.5066(8) -0.3210(5) -0.5296(16) 0.060(3) Uani 0.384(8) 1 d DG U P A 1
C14 C -0.4100(10) -0.3183(11) -0.513(3) 0.053(6) Uani 0.384(8) 1 d DG U P A 1
C15 C -0.3586(12) -0.3894(16) -0.506(3) 0.053(5) Uani 0.384(8) 1 d DG U P A 1
C16 C -0.4038(19) -0.4631(11) -0.516(4) 0.053(8) Uani 0.384(8) 1 d DG U P A 1
F1 F -0.6461(4) -0.3979(3) -0.5253(9) 0.0559(15) Uani 0.384(8) 1 d D U P A 1
F2 F -0.565(7) -0.256(4) -0.517(6) 0.055(7) Uani 0.384(8) 1 d D U P A 1
F3 F -0.373(2) -0.2448(13) -0.491(2) 0.065(5) Uani 0.384(8) 1 d D U P A 1
F4 F -0.2679(14) -0.3793(14) -0.4849(18) 0.064(4) Uani 0.384(8) 1 d D U P A 1
F5 F -0.350(3) -0.5306(19) -0.506(3) 0.059(5) Uani 0.384(8) 1 d D U P A 1
C21 C -0.746(2) -0.7170(18) -0.706(2) 0.054(5) Uani 0.384(8) 1 d D U P A 1
C22 C -0.6819(19) -0.781(2) -0.749(2) 0.048(5) Uani 0.384(8) 1 d D U P A 1
H22A H -0.6463 -0.7562 -0.7961 0.058 Uiso 0.384(8) 1 calc R U P A 1
H22B H -0.6359 -0.8023 -0.7075 0.058 Uiso 0.384(8) 1 calc R U P A 1
C23 C -0.805(2) -0.754(2) -0.6360(18) 0.056(5) Uani 0.384(8) 1 d D U P A 1
H23A H -0.8452 -0.7123 -0.6095 0.067 Uiso 0.384(8) 1 calc R U P A 1
H23B H -0.7631 -0.7767 -0.5919 0.067 Uiso 0.384(8) 1 calc R U P A 1
C24 C -0.813(2) -0.6813(18) -0.774(2) 0.061(5) Uani 0.384(8) 1 d D U P A 1
H24A H -0.8529 -0.6387 -0.7490 0.073 Uiso 0.384(8) 1 calc R U P A 1
H24B H -0.7754 -0.6569 -0.8205 0.073 Uiso 0.384(8) 1 calc R U P A 1
C25 C -0.744(2) -0.8497(19) -0.783(2) 0.062(5) Uani 0.384(8) 1 d D U P A 1
H25 H -0.7038 -0.8921 -0.8097 0.075 Uiso 0.384(8) 1 calc R U P A 1
C26 C -0.801(3) -0.8849(19) -0.712(3) 0.060(4) Uani 0.384(8) 1 d D U P A 1
H26A H -0.7574 -0.9056 -0.6675 0.072 Uiso 0.384(8) 1 calc R U P A 1
H26B H -0.8385 -0.9307 -0.7331 0.072 Uiso 0.384(8) 1 calc R U P A 1
C27 C -0.868(2) -0.821(2) -0.672(2) 0.056(5) Uani 0.384(8) 1 d D U P A 1
H27 H -0.9063 -0.8462 -0.6257 0.067 Uiso 0.384(8) 1 calc R U P A 1
C28 C -0.9334(19) -0.788(2) -0.739(2) 0.060(5) Uani 0.384(8) 1 d D U P A 1
H28A H -0.9765 -0.7477 -0.7135 0.072 Uiso 0.384(8) 1 calc R U P A 1
H28B H -0.9725 -0.8319 -0.7627 0.072 Uiso 0.384(8) 1 calc R U P A 1
C29 C -0.876(2) -0.748(2) -0.810(2) 0.061(5) Uani 0.384(8) 1 d D U P A 1
H29 H -0.9202 -0.7254 -0.8540 0.074 Uiso 0.384(8) 1 calc R U P A 1
C30 C -0.814(2) -0.812(2) -0.8492(19) 0.063(5) Uani 0.384(8) 1 d D U P A 1
H30A H -0.7765 -0.7874 -0.8958 0.076 Uiso 0.384(8) 1 calc R U P A 1
H30B H -0.8538 -0.8547 -0.8736 0.076 Uiso 0.384(8) 1 calc R U P A 1
C31 C -0.700(2) -0.728(2) -0.3143(19) 0.047(5) Uani 0.384(8) 1 d D U P A 1
C32 C -0.652(2) -0.812(3) -0.316(3) 0.067(5) Uani 0.384(8) 1 d D U P A 1
H32A H -0.6369 -0.8269 -0.3752 0.080 Uiso 0.384(8) 1 calc R U P A 1
H32B H -0.5927 -0.8105 -0.2834 0.080 Uiso 0.384(8) 1 calc R U P A 1
C33 C -0.727(3) -0.708(2) -0.2233(19) 0.076(6) Uani 0.384(8) 1 d D U P A 1
H33A H -0.7549 -0.6532 -0.2211 0.091 Uiso 0.384(8) 1 calc R U P A 1
H33B H -0.6690 -0.7077 -0.1879 0.091 Uiso 0.384(8) 1 calc R U P A 1
C34 C -0.790(2) -0.731(2) -0.371(2) 0.048(5) Uani 0.384(8) 1 d D U P A 1
H34A H -0.8202 -0.6766 -0.3722 0.058 Uiso 0.384(8) 1 calc R U P A 1
H34B H -0.7730 -0.7459 -0.4289 0.058 Uiso 0.384(8) 1 calc R U P A 1
C35 C -0.720(3) -0.874(2) -0.278(3) 0.075(5) Uani 0.384(8) 1 d D U P A 1
H35 H -0.6900 -0.9280 -0.2797 0.090 Uiso 0.384(8) 1 calc R U P A 1
C36 C -0.747(3) -0.853(3) -0.189(2) 0.092(7) Uani 0.384(8) 1 d D U P A 1
H36A H -0.6904 -0.8512 -0.1526 0.111 Uiso 0.384(8) 1 calc R U P A 1
H36B H -0.7905 -0.8949 -0.1663 0.111 Uiso 0.384(8) 1 calc R U P A 1
C37 C -0.798(3) -0.770(2) -0.188(2) 0.088(7) Uani 0.384(8) 1 d D U P A 1
H37 H -0.8158 -0.7548 -0.1288 0.106 Uiso 0.384(8) 1 calc R U P A 1
C38 C -0.884(2) -0.769(3) -0.243(3) 0.088(7) Uani 0.384(8) 1 d D U P A 1
H38A H -0.9135 -0.7152 -0.2423 0.106 Uiso 0.384(8) 1 calc R U P A 1
H38B H -0.9313 -0.8081 -0.2203 0.106 Uiso 0.384(8) 1 calc R U P A 1
C39 C -0.860(2) -0.792(2) -0.334(2) 0.063(5) Uani 0.384(8) 1 d D U P A 1
H39 H -0.9188 -0.7942 -0.3688 0.076 Uiso 0.384(8) 1 calc R U P A 1
C40 C -0.812(3) -0.874(2) -0.333(3) 0.067(6) Uani 0.384(8) 1 d D U P A 1
H40A H -0.7958 -0.8890 -0.3919 0.081 Uiso 0.384(8) 1 calc R U P A 1
H40B H -0.8564 -0.9145 -0.3108 0.081 Uiso 0.384(8) 1 calc R U P A 1
N3 N -0.5857(6) -0.8266(4) -0.5251(13) 0.051(2) Uani 0.338(15) 1 d D U P A 1
C41 C -0.538(2) -0.9037(15) -0.535(2) 0.060(3) Uani 0.338(15) 1 d D U P A 1
C42 C -0.514(3) -0.922(2) -0.629(2) 0.066(5) Uani 0.338(15) 1 d D U P A 1
H42A H -0.5735 -0.9240 -0.6620 0.079 Uiso 0.338(15) 1 calc R U P A 1
H42B H -0.4744 -0.8783 -0.6515 0.079 Uiso 0.338(15) 1 calc R U P A 1
C43 C -0.448(3) -0.901(2) -0.483(3) 0.068(5) Uani 0.338(15) 1 d D U P A 1
H43A H -0.4633 -0.8899 -0.4227 0.082 Uiso 0.338(15) 1 calc R U P A 1
H43B H -0.4060 -0.8580 -0.5036 0.082 Uiso 0.338(15) 1 calc R U P A 1
C44 C -0.604(2) -0.972(2) -0.503(3) 0.063(5) Uani 0.338(15) 1 d D U P A 1
H44A H -0.6221 -0.9613 -0.4431 0.076 Uiso 0.338(15) 1 calc R U P A 1
H44B H -0.6630 -0.9726 -0.5368 0.076 Uiso 0.338(15) 1 calc R U P A 1
C45 C -0.462(3) -1.002(2) -0.637(2) 0.079(6) Uani 0.338(15) 1 d D U P A 1
H45 H -0.4465 -1.0126 -0.6978 0.094 Uiso 0.338(15) 1 calc R U P A 1
C46 C -0.375(2) -1.000(2) -0.584(3) 0.075(6) Uani 0.338(15) 1 d D U P A 1
H46A H -0.3313 -0.9580 -0.6054 0.090 Uiso 0.338(15) 1 calc R U P A 1
H46B H -0.3417 -1.0527 -0.5890 0.090 Uiso 0.338(15) 1 calc R U P A 1
C47 C -0.398(2) -0.984(2) -0.490(3) 0.075(6) Uani 0.338(15) 1 d D U P A 1
H47 H -0.3384 -0.9831 -0.4564 0.090 Uiso 0.338(15) 1 calc R U P A 1
C48 C -0.464(3) -1.049(2) -0.457(3) 0.084(6) Uani 0.338(15) 1 d D U P A 1
H48A H -0.4798 -1.0368 -0.3973 0.101 Uiso 0.338(15) 1 calc R U P A 1
H48B H -0.4306 -1.1011 -0.4585 0.101 Uiso 0.338(15) 1 calc R U P A 1
C49 C -0.554(2) -1.0535(18) -0.509(3) 0.080(6) Uani 0.338(15) 1 d D U P A 1
H49 H -0.5960 -1.0972 -0.4871 0.096 Uiso 0.338(15) 1 calc R U P A 1
C50 C -0.528(3) -1.070(2) -0.601(3) 0.092(7) Uani 0.338(15) 1 d D U P A 1
H50A H -0.5864 -1.0735 -0.6350 0.110 Uiso 0.338(15) 1 calc R U P A 1
H50B H -0.4948 -1.1223 -0.6045 0.110 Uiso 0.338(15) 1 calc R U P A 1
C1A C -0.540(2) -0.5515(14) -0.5255(14) 0.038(7) Uani 0.616(8) 1 d D . P A 2
N1A N -0.6050(19) -0.6542(14) -0.6172(14) 0.047(7) Uani 0.616(8) 1 d D . P A 2
C2A C -0.5532(19) -0.5824(16) -0.6057(14) 0.045(7) Uani 0.616(8) 1 d D . P A 2
C3A C -0.543(2) -0.5447(18) -0.6845(18) 0.065(7) Uani 0.616(8) 1 d D . P A 2
H3A H -0.5139 -0.4939 -0.6943 0.079 Uiso 0.616(8) 1 calc R U P A 2
C4A C -0.5810(19) -0.5929(16) -0.7442(16) 0.061(6) Uani 0.616(8) 1 d D . P A 2
H4A H -0.5802 -0.5842 -0.8035 0.073 Uiso 0.616(8) 1 calc R U P A 2
C5A C -0.622(2) -0.6585(16) -0.7019(15) 0.049(5) Uani 0.616(8) 1 d D . P A 2
N2A N -0.634(2) -0.6483(12) -0.4440(12) 0.034(7) Uani 0.616(8) 1 d D . P A 2
C6A C -0.5770(12) -0.5788(11) -0.4498(10) 0.046(4) Uani 0.616(8) 1 d D . P A 2
C7A C -0.5886(15) -0.5327(17) -0.3730(15) 0.048(7) Uani 0.616(8) 1 d D . P A 2
H7A H -0.5630 -0.4812 -0.3608 0.058 Uiso 0.616(8) 1 calc R U P A 2
C8A C -0.6464(17) -0.5807(16) -0.3197(15) 0.055(8) Uani 0.616(8) 1 d D . P A 2
H8A H -0.6654 -0.5674 -0.2639 0.067 Uiso 0.616(8) 1 calc R U P A 2
C9A C -0.6710(15) -0.6514(17) -0.3634(14) 0.044(5) Uani 0.616(8) 1 d D . P A 2
C11A C -0.4997(17) -0.4660(9) -0.534(4) 0.048(3) Uani 0.616(8) 1 d . . P A 2
C12A C -0.5502(11) -0.3958(9) -0.521(3) 0.044(6) Uani 0.616(8) 1 d D . P A 2
C13A C -0.5066(8) -0.3210(5) -0.5296(16) 0.060(3) Uani 0.616(8) 1 d D . P A 2
C14A C -0.4119(15) -0.3149(11) -0.547(2) 0.053(6) Uani 0.616(8) 1 d D . P A 2
C15A C -0.3578(14) -0.3829(13) -0.549(2) 0.053(5) Uani 0.616(8) 1 d D . P A 2
C16A C -0.4046(18) -0.4565(11) -0.543(3) 0.053(8) Uani 0.616(8) 1 d D . P A 2
F1A F -0.6461(4) -0.3979(3) -0.5253(9) 0.0559(15) Uani 0.616(8) 1 d D . P A 2
F2A F -0.557(4) -0.251(2) -0.537(3) 0.055(7) Uani 0.616(8) 1 d D . P A 2
F3A F -0.3638(11) -0.2437(7) -0.5413(13) 0.065(5) Uani 0.616(8) 1 d D . P A 2
F4A F -0.2607(9) -0.3814(8) -0.5457(11) 0.064(4) Uani 0.616(8) 1 d D . P A 2
F5A F -0.3472(16) -0.5227(11) -0.5438(14) 0.059(5) Uani 0.616(8) 1 d D . P A 2
C21A C -0.6850(15) -0.7225(12) -0.7414(13) 0.054(5) Uani 0.616(8) 1 d D . P A 2
C22A C -0.6385(15) -0.8062(12) -0.7376(16) 0.048(5) Uani 0.616(8) 1 d D . P A 2
H22C H -0.5799 -0.8057 -0.7719 0.058 Uiso 0.616(8) 1 calc R U P A 2
H22D H -0.6206 -0.8181 -0.6784 0.058 Uiso 0.616(8) 1 calc R U P A 2
C23A C -0.7785(16) -0.7251(15) -0.6939(15) 0.056(5) Uani 0.616(8) 1 d D . P A 2
H23C H -0.8096 -0.6719 -0.6982 0.067 Uiso 0.616(8) 1 calc R U P A 2
H23D H -0.7659 -0.7358 -0.6334 0.067 Uiso 0.616(8) 1 calc R U P A 2
C24A C -0.7088(17) -0.7012(14) -0.8348(12) 0.061(5) Uani 0.616(8) 1 d D . P A 2
H24C H -0.7414 -0.6485 -0.8375 0.073 Uiso 0.616(8) 1 calc R U P A 2
H24D H -0.6500 -0.6977 -0.8685 0.073 Uiso 0.616(8) 1 calc R U P A 2
C25A C -0.7038(15) -0.8723(13) -0.7700(16) 0.062(5) Uani 0.616(8) 1 d D . P A 2
H25A H -0.6721 -0.9260 -0.7671 0.075 Uiso 0.616(8) 1 calc R U P A 2
C26A C -0.7945(19) -0.8726(14) -0.7206(18) 0.060(4) Uani 0.616(8) 1 d D . P A 2
H26C H -0.7808 -0.8842 -0.6605 0.072 Uiso 0.616(8) 1 calc R U P A 2
H26D H -0.8366 -0.9155 -0.7423 0.072 Uiso 0.616(8) 1 calc R U P A 2
C27A C -0.8451(15) -0.7896(14) -0.7281(13) 0.056(5) Uani 0.616(8) 1 d D . P A 2
H27A H -0.9054 -0.7900 -0.6950 0.067 Uiso 0.616(8) 1 calc R U P A 2
C28A C -0.8658(15) -0.7731(17) -0.8206(15) 0.060(5) Uani 0.616(8) 1 d D . P A 2
H28C H -0.9016 -0.7221 -0.8261 0.072 Uiso 0.616(8) 1 calc R U P A 2
H28D H -0.9050 -0.8170 -0.8441 0.072 Uiso 0.616(8) 1 calc R U P A 2
C29A C -0.7728(14) -0.7670(14) -0.8701(13) 0.061(5) Uani 0.616(8) 1 d D . P A 2
H29A H -0.7874 -0.7547 -0.9306 0.074 Uiso 0.616(8) 1 calc R U P A 2
C30A C -0.7270(15) -0.8488(14) -0.8648(13) 0.063(5) Uani 0.616(8) 1 d D . P A 2
H30C H -0.6678 -0.8488 -0.8983 0.076 Uiso 0.616(8) 1 calc R U P A 2
H30D H -0.7700 -0.8896 -0.8895 0.076 Uiso 0.616(8) 1 calc R U P A 2
C31A C -0.7321(14) -0.7215(14) -0.3376(12) 0.047(5) Uani 0.616(8) 1 d D . P A 2
C32A C -0.6702(16) -0.7932(15) -0.308(2) 0.067(5) Uani 0.616(8) 1 d D . P A 2
H32C H -0.6285 -0.8105 -0.3552 0.080 Uiso 0.616(8) 1 calc R U P A 2
H32D H -0.6296 -0.7762 -0.2606 0.080 Uiso 0.616(8) 1 calc R U P A 2
C33A C -0.7974(17) -0.6968(15) -0.2661(14) 0.076(6) Uani 0.616(8) 1 d D . P A 2
H33C H -0.8375 -0.6513 -0.2847 0.091 Uiso 0.616(8) 1 calc R U P A 2
H33D H -0.7592 -0.6786 -0.2173 0.091 Uiso 0.616(8) 1 calc R U P A 2
C34A C -0.7948(16) -0.7506(14) -0.4125(13) 0.048(5) Uani 0.616(8) 1 d D . P A 2
H34C H -0.8357 -0.7058 -0.4317 0.058 Uiso 0.616(8) 1 calc R U P A 2
H34D H -0.7538 -0.7666 -0.4603 0.058 Uiso 0.616(8) 1 calc R U P A 2
C35A C -0.7324(18) -0.8632(16) -0.2809(18) 0.075(5) Uani 0.616(8) 1 d D . P A 2
H35A H -0.6914 -0.9086 -0.2616 0.090 Uiso 0.616(8) 1 calc R U P A 2
C36A C -0.7959(19) -0.8376(17) -0.2097(16) 0.092(7) Uani 0.616(8) 1 d D . P A 2
H36C H -0.7572 -0.8201 -0.1609 0.111 Uiso 0.616(8) 1 calc R U P A 2
H36D H -0.8355 -0.8836 -0.1915 0.111 Uiso 0.616(8) 1 calc R U P A 2
C37A C -0.8604(19) -0.7673(19) -0.2394(17) 0.088(7) Uani 0.616(8) 1 d D . P A 2
H37A H -0.9031 -0.7503 -0.1923 0.106 Uiso 0.616(8) 1 calc R U P A 2
C38A C -0.9186(16) -0.7947(19) -0.3144(17) 0.088(7) Uani 0.616(8) 1 d D . P A 2
H38C H -0.9602 -0.8396 -0.2969 0.106 Uiso 0.616(8) 1 calc R U P A 2
H38D H -0.9593 -0.7498 -0.3337 0.106 Uiso 0.616(8) 1 calc R U P A 2
C39A C -0.8565(16) -0.8219(15) -0.3863(15) 0.063(5) Uani 0.616(8) 1 d D . P A 2
H39A H -0.8967 -0.8392 -0.4351 0.076 Uiso 0.616(8) 1 calc R U P A 2
C40A C -0.793(2) -0.8912(15) -0.3586(16) 0.067(6) Uani 0.616(8) 1 d D . P A 2
H40C H -0.7503 -0.9070 -0.4056 0.081 Uiso 0.616(8) 1 calc R U P A 2
H40D H -0.8316 -0.9384 -0.3429 0.081 Uiso 0.616(8) 1 calc R U P A 2
N3A N -0.5857(6) -0.8266(4) -0.5251(13) 0.051(2) Uani 0.662(15) 1 d D . P A 2
C41A C -0.5353(14) -0.9025(9) -0.5330(16) 0.060(3) Uani 0.662(15) 1 d D . P A 2
C42A C -0.4485(15) -0.8945(12) -0.5929(16) 0.066(5) Uani 0.662(15) 1 d D . P A
2
H42C H -0.4705 -0.8797 -0.6502 0.079 Uiso 0.662(15) 1 calc R U P A 2
H42D H -0.4067 -0.8509 -0.5722 0.079 Uiso 0.662(15) 1 calc R U P A 2
C43A C -0.5022(18) -0.9247(13) -0.4453(14) 0.068(5) Uani 0.662(15) 1 d D . P A
2
H43C H -0.5574 -0.9301 -0.4072 0.082 Uiso 0.662(15) 1 calc R U P A 2
H43D H -0.4607 -0.8817 -0.4228 0.082 Uiso 0.662(15) 1 calc R U P A 2
C44A C -0.6009(14) -0.9699(12) -0.5683(18) 0.063(5) Uani 0.662(15) 1 d D . P A
2
H44C H -0.6568 -0.9764 -0.5312 0.076 Uiso 0.662(15) 1 calc R U P A 2
H44D H -0.6233 -0.9551 -0.6255 0.076 Uiso 0.662(15) 1 calc R U P A 2
C45A C -0.3926(16) -0.9727(12) -0.5976(16) 0.079(6) Uani 0.662(15) 1 d D . P A
2
H45A H -0.3364 -0.9664 -0.6354 0.094 Uiso 0.662(15) 1 calc R U P A 2
C46A C -0.3628(13) -0.9961(11) -0.5111(15) 0.075(6) Uani 0.662(15) 1 d D . P A
2
H46C H -0.3183 -0.9552 -0.4890 0.090 Uiso 0.662(15) 1 calc R U P A 2
H46D H -0.3286 -1.0480 -0.5139 0.090 Uiso 0.662(15) 1 calc R U P A 2
C47A C -0.4475(15) -1.0045(13) -0.4486(15) 0.075(6) Uani 0.662(15) 1 d D . P A
2
H47A H -0.4243 -1.0194 -0.3911 0.090 Uiso 0.662(15) 1 calc R U P A 2
C48A C -0.5118(18) -1.0693(13) -0.4827(17) 0.084(6) Uani 0.662(15) 1 d D . P A
2
H48C H -0.5675 -1.0748 -0.4453 0.101 Uiso 0.662(15) 1 calc R U P A 2
H48D H -0.4777 -1.1213 -0.4830 0.101 Uiso 0.662(15) 1 calc R U P A 2
C49A C -0.5449(15) -1.0498(12) -0.5723(18) 0.080(6) Uani 0.662(15) 1 d D . P A
2
H49A H -0.5871 -1.0938 -0.5932 0.096 Uiso 0.662(15) 1 calc R U P A 2
C50A C -0.4617(17) -1.0391(14) -0.6328(17) 0.092(7) Uani 0.662(15) 1 d D . P A
2
H50C H -0.4853 -1.0230 -0.6891 0.110 Uiso 0.662(15) 1 calc R U P A 2
H50D H -0.4273 -1.0907 -0.6388 0.110 Uiso 0.662(15) 1 calc R U P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0677(12) 0.0326(8) 0.0390(9) 0.0025(19) 0.0064(18) 0.0040(8)
C1 0.034(17) 0.026(10) 0.051(7) -0.002(7) 0.006(8) 0.019(11)
N1 0.070(17) 0.028(6) 0.041(7) 0.001(6) -0.001(9) 0.005(8)
C2 0.058(17) 0.029(8) 0.048(6) 0.007(6) -0.001(9) 0.009(9)
C3 0.088(17) 0.044(9) 0.064(9) 0.024(7) -0.015(11) -0.005(10)
C4 0.076(14) 0.057(9) 0.049(9) 0.021(7) -0.008(9) -0.007(9)
C5 0.062(11) 0.042(7) 0.042(8) 0.004(6) 0.000(7) 0.002(7)
N2 0.029(16) 0.034(6) 0.040(6) -0.001(5) -0.003(7) 0.008(7)
C6 0.054(9) 0.035(6) 0.049(6) -0.008(5) 0.003(6) 0.000(6)
C7 0.037(18) 0.055(11) 0.054(7) -0.019(7) 0.001(8) 0.010(11)
C8 0.04(2) 0.072(11) 0.051(8) -0.021(7) 0.006(9) 0.000(12)
C9 0.028(12) 0.060(9) 0.043(7) -0.001(6) 0.004(7) 0.008(8)
C11 0.060(5) 0.034(4) 0.048(8) 0.001(6) 0.004(6) -0.002(3)
C12 0.065(6) 0.035(4) 0.031(16) 0.004(7) 0.002(7) 0.003(4)
C13 0.074(6) 0.031(4) 0.074(8) 0.001(8) 0.008(8) 0.006(4)
C14 0.073(6) 0.029(4) 0.058(19) 0.010(8) 0.018(8) -0.001(4)
C15 0.061(6) 0.040(5) 0.056(14) 0.011(8) 0.025(8) -0.003(4)
C16 0.064(6) 0.027(5) 0.07(3) 0.016(8) 0.007(8) 0.004(4)
F1 0.071(4) 0.043(3) 0.053(4) 0.014(7) 0.005(6) 0.004(3)
F2 0.085(10) 0.034(6) 0.05(2) 0.003(9) 0.011(12) 0.005(7)
F3 0.085(6) 0.036(3) 0.074(15) -0.003(9) 0.030(10) -0.009(3)
F4 0.063(5) 0.047(4) 0.080(11) 0.012(8) 0.023(7) -0.005(3)
F5 0.065(5) 0.035(5) 0.078(14) 0.012(9) 0.009(10) 0.002(4)
C21 0.059(9) 0.059(8) 0.043(8) -0.013(6) 0.002(6) -0.001(7)
C22 0.044(10) 0.060(9) 0.041(10) -0.016(8) 0.002(7) -0.002(7)
C23 0.064(11) 0.053(9) 0.050(9) -0.015(7) 0.011(7) 0.002(8)
C24 0.056(10) 0.081(10) 0.046(9) -0.008(7) 0.002(7) -0.002(7)
C25 0.045(11) 0.069(10) 0.073(10) -0.029(8) -0.001(8) -0.005(7)
C26 0.044(9) 0.064(9) 0.071(9) -0.032(7) 0.004(7) -0.009(7)
C27 0.053(9) 0.063(10) 0.051(10) -0.020(7) 0.004(7) 0.003(7)
C28 0.046(9) 0.089(13) 0.046(9) -0.016(8) 0.012(7) 0.008(8)
C29 0.050(10) 0.090(11) 0.045(9) -0.020(7) 0.010(7) 0.004(7)
C30 0.042(10) 0.094(11) 0.053(9) -0.037(8) 0.001(7) 0.002(8)
C31 0.044(10) 0.073(9) 0.025(9) -0.003(6) 0.006(7) -0.008(7)
C32 0.068(11) 0.081(10) 0.051(11) 0.008(8) 0.013(8) 0.001(8)
C33 0.064(13) 0.124(14) 0.038(9) -0.011(8) 0.015(7) -0.022(10)
C34 0.046(9) 0.059(11) 0.040(11) -0.007(8) 0.001(8) 0.000(7)
C35 0.071(10) 0.092(11) 0.063(9) 0.028(8) 0.015(7) 0.000(8)
C36 0.059(17) 0.150(15) 0.068(11) 0.016(9) 0.027(9) -0.027(11)
C37 0.064(13) 0.138(15) 0.064(12) 0.008(9) 0.025(8) -0.021(10)
C38 0.070(12) 0.118(16) 0.076(11) -0.011(10) 0.019(9) -0.013(10)
C39 0.054(10) 0.068(11) 0.068(12) 0.004(8) 0.007(8) -0.005(8)
C40 0.067(11) 0.075(11) 0.060(13) 0.019(8) 0.018(9) -0.002(8)
N3 0.066(6) 0.035(4) 0.054(5) 0.005(6) 0.014(9) 0.013(3)
C41 0.056(6) 0.027(4) 0.099(8) -0.004(7) 0.006(7) 0.007(4)
C42 0.051(11) 0.045(9) 0.101(10) -0.011(7) 0.011(8) 0.009(7)
C43 0.054(9) 0.046(9) 0.105(13) 0.008(8) -0.004(9) 0.003(7)
C44 0.043(7) 0.032(5) 0.116(14) -0.001(9) 0.005(10) 0.006(5)
C45 0.062(10) 0.046(10) 0.128(13) -0.015(8) 0.008(9) 0.015(7)
C46 0.063(10) 0.033(7) 0.130(14) 0.005(9) 0.010(9) 0.000(6)
C47 0.050(11) 0.039(9) 0.136(14) 0.006(8) 0.001(8) 0.004(7)
C48 0.053(12) 0.038(10) 0.162(15) 0.020(9) 0.010(10) -0.001(8)
C49 0.052(10) 0.034(7) 0.154(15) -0.007(9) 0.017(10) 0.005(6)
C50 0.071(13) 0.045(10) 0.159(15) -0.007(9) 0.023(10) 0.017(8)
C1A 0.039(17) 0.024(10) 0.051(10) -0.006(17) -0.003(17) 0.013(11)
N1A 0.070(17) 0.028(6) 0.041(7) 0.001(6) -0.001(9) 0.005(8)
C2A 0.058(17) 0.029(8) 0.048(6) 0.007(6) -0.001(9) 0.009(9)
C3A 0.088(17) 0.044(9) 0.064(9) 0.024(7) -0.015(11) -0.005(10)
C4A 0.076(14) 0.057(9) 0.049(9) 0.021(7) -0.008(9) -0.007(9)
C5A 0.062(11) 0.042(7) 0.042(8) 0.004(6) 0.000(7) 0.002(7)
N2A 0.029(16) 0.034(6) 0.040(6) -0.001(5) -0.003(7) 0.008(7)
C6A 0.054(9) 0.035(6) 0.049(6) -0.008(5) 0.003(6) 0.000(6)
C7A 0.037(18) 0.055(11) 0.054(7) -0.019(7) 0.001(8) 0.010(11)
C8A 0.04(2) 0.072(11) 0.051(8) -0.021(7) 0.006(9) 0.000(12)
C9A 0.028(12) 0.060(9) 0.043(7) -0.001(6) 0.004(7) 0.008(8)
C11A 0.060(5) 0.034(4) 0.048(8) 0.001(6) 0.004(6) -0.002(3)
C12A 0.065(6) 0.035(4) 0.031(16) 0.004(7) 0.002(7) 0.003(4)
C13A 0.074(6) 0.031(4) 0.074(8) 0.001(8) 0.008(8) 0.006(4)
C14A 0.073(6) 0.029(4) 0.058(19) 0.010(8) 0.018(8) -0.001(4)
C15A 0.061(6) 0.040(5) 0.056(14) 0.011(8) 0.025(8) -0.003(4)
C16A 0.064(6) 0.027(5) 0.07(3) 0.016(8) 0.007(8) 0.004(4)
F1A 0.071(4) 0.043(3) 0.053(4) 0.014(7) 0.005(6) 0.004(3)
F2A 0.085(10) 0.034(6) 0.05(2) 0.003(9) 0.011(12) 0.005(7)
F3A 0.085(6) 0.036(3) 0.074(15) -0.003(9) 0.030(10) -0.009(3)
F4A 0.063(5) 0.047(4) 0.080(11) 0.012(8) 0.023(7) -0.005(3)
F5A 0.065(5) 0.035(5) 0.078(14) 0.012(9) 0.009(10) 0.002(4)
C21A 0.059(9) 0.059(8) 0.043(8) -0.013(6) 0.002(6) -0.001(7)
C22A 0.044(10) 0.060(9) 0.041(10) -0.016(8) 0.002(7) -0.002(7)
C23A 0.064(11) 0.053(9) 0.050(9) -0.015(7) 0.011(7) 0.002(8)
C24A 0.056(10) 0.081(10) 0.046(9) -0.008(7) 0.002(7) -0.002(7)
C25A 0.045(11) 0.069(10) 0.073(10) -0.029(8) -0.001(8) -0.005(7)
C26A 0.044(9) 0.064(9) 0.071(9) -0.032(7) 0.004(7) -0.009(7)
C27A 0.053(9) 0.063(10) 0.051(10) -0.020(7) 0.004(7) 0.003(7)
C28A 0.046(9) 0.089(13) 0.046(9) -0.016(8) 0.012(7) 0.008(8)
C29A 0.050(10) 0.090(11) 0.045(9) -0.020(7) 0.010(7) 0.004(7)
C30A 0.042(10) 0.094(11) 0.053(9) -0.037(8) 0.001(7) 0.002(8)
C31A 0.044(10) 0.073(9) 0.025(9) -0.003(6) 0.006(7) -0.008(7)
C32A 0.068(11) 0.081(10) 0.051(11) 0.008(8) 0.013(8) 0.001(8)
C33A 0.064(13) 0.124(14) 0.038(9) -0.011(8) 0.015(7) -0.022(10)
C34A 0.046(9) 0.059(11) 0.040(11) -0.007(8) 0.001(8) 0.000(7)
C35A 0.071(10) 0.092(11) 0.063(9) 0.028(8) 0.015(7) 0.000(8)
C36A 0.059(17) 0.150(15) 0.068(11) 0.016(9) 0.027(9) -0.027(11)
C37A 0.064(13) 0.138(15) 0.064(12) 0.008(9) 0.025(8) -0.021(10)
C38A 0.070(12) 0.118(16) 0.076(11) -0.011(10) 0.019(9) -0.013(10)
C39A 0.054(10) 0.068(11) 0.068(12) 0.004(8) 0.007(8) -0.005(8)
C40A 0.067(11) 0.075(11) 0.060(13) 0.019(8) 0.018(9) -0.002(8)
N3A 0.066(6) 0.035(4) 0.054(5) 0.005(6) 0.014(9) 0.013(3)
C41A 0.056(6) 0.027(4) 0.099(8) -0.004(7) 0.006(7) 0.007(4)
C42A 0.051(11) 0.045(9) 0.101(10) -0.011(7) 0.011(8) 0.009(7)
C43A 0.054(9) 0.046(9) 0.105(13) 0.008(8) -0.004(9) 0.003(7)
C44A 0.043(7) 0.032(5) 0.116(14) -0.001(9) 0.005(10) 0.006(5)
C45A 0.062(10) 0.046(10) 0.128(13) -0.015(8) 0.008(9) 0.015(7)
C46A 0.063(10) 0.033(7) 0.130(14) 0.005(9) 0.010(9) 0.000(6)
C47A 0.050(11) 0.039(9) 0.136(14) 0.006(8) 0.001(8) 0.004(7)
C48A 0.053(12) 0.038(10) 0.162(15) 0.020(9) 0.010(10) -0.001(8)
C49A 0.052(10) 0.034(7) 0.154(15) -0.007(9) 0.017(10) 0.005(6)
C50A 0.071(13) 0.045(10) 0.159(15) -0.007(9) 0.023(10) 0.017(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3A 1.642(7) . ?
Ni1 N3 1.642(7) . ?
Ni1 N2 1.89(2) . ?
Ni1 N2A 1.903(19) . ?
Ni1 N1 1.91(2) . ?
Ni1 N1A 1.929(19) . ?
C1 C2 1.38(2) . ?
C1 C6 1.38(2) . ?
C1 C11 1.48(4) . ?
N1 C5 1.34(3) . ?
N1 C2 1.41(3) . ?
C2 C3 1.41(3) . ?
C3 C4 1.33(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.41(4) . ?
C4 H4 0.9500 . ?
C5 C21 1.52(3) . ?
N2 C9 1.39(3) . ?
N2 C6 1.41(3) . ?
C6 C7 1.45(3) . ?
C7 C8 1.44(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.41(4) . ?
C8 H8 0.9500 . ?
C9 C31 1.52(4) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 F1 1.35(2) . ?
C12 C13 1.3900 . ?
C13 F2 1.37(2) . ?
C13 C14 1.3900 . ?
C14 F3 1.37(2) . ?
C14 C15 1.3900 . ?
C15 F4 1.34(2) . ?
C15 C16 1.3900 . ?
C16 F5 1.37(2) . ?
C21 C23 1.53(3) . ?
C21 C22 1.55(2) . ?
C21 C24 1.56(2) . ?
C22 C25 1.53(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C27 1.54(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C29 1.53(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.50(3) . ?
C25 C30 1.58(3) . ?
C25 H25 1.0000 . ?
C26 C27 1.56(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.51(3) . ?
C27 H27 1.0000 . ?
C28 C29 1.54(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.51(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C33 1.53(2) . ?
C31 C34 1.55(2) . ?
C31 C32 1.55(2) . ?
C32 C35 1.52(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C37 1.54(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C39 1.54(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.51(3) . ?
C35 C40 1.57(3) . ?
C35 H35 1.0000 . ?
C36 C37 1.56(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.50(3) . ?
C37 H37 1.0000 . ?
C38 C39 1.52(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.52(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
N3 C41 1.45(2) . ?
C41 C43 1.52(3) . ?
C41 C44 1.55(2) . ?
C41 C42 1.56(2) . ?
C42 C45 1.52(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C47 1.55(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C49 1.54(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.50(3) . ?
C45 C50 1.58(3) . ?
C45 H45 1.0000 . ?
C46 C47 1.55(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.52(3) . ?
C47 H47 1.0000 . ?
C48 C49 1.53(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.52(3) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C1A C2A 1.382(18) . ?
C1A C6A 1.384(18) . ?
C1A C11A 1.54(3) . ?
N1A C5A 1.36(3) . ?
N1A C2A 1.41(3) . ?
C2A C3A 1.40(3) . ?
C3A C4A 1.35(3) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.41(3) . ?
C4A H4A 0.9500 . ?
C5A C21A 1.52(3) . ?
N2A C9A 1.38(2) . ?
N2A C6A 1.41(3) . ?
C6A C7A 1.45(3) . ?
C7A C8A 1.42(3) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.41(3) . ?
C8A H8A 0.9500 . ?
C9A C31A 1.51(3) . ?
C11A C16A 1.36(3) . ?
C11A C12A 1.38(2) . ?
C12A F1A 1.357(16) . ?
C12A C13A 1.39(2) . ?
C13A F2A 1.367(17) . ?
C13A C14A 1.37(2) . ?
C14A C15A 1.36(2) . ?
C14A F3A 1.368(17) . ?
C15A F4A 1.373(19) . ?
C15A C16A 1.39(2) . ?
C16A F5A 1.368(16) . ?
C21A C23A 1.52(2) . ?
C21A C22A 1.538(19) . ?
C21A C24A 1.56(2) . ?
C22A C25A 1.525(18) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A C27A 1.53(2) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A C29A 1.52(2) . ?
C24A H24C 0.9900 . ?
C24A H24D 0.9900 . ?
C25A C26A 1.50(2) . ?
C25A C30A 1.58(3) . ?
C25A H25A 1.0000 . ?
C26A C27A 1.56(2) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C27A C28A 1.52(2) . ?
C27A H27A 1.0000 . ?
C28A C29A 1.53(2) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C29A C30A 1.51(2) . ?
C29A H29A 1.0000 . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C31A C33A 1.52(2) . ?
C31A C32A 1.55(2) . ?
C31A C34A 1.56(2) . ?
C32A C35A 1.521(19) . ?
C32A H32C 0.9900 . ?
C32A H32D 0.9900 . ?
C33A C37A 1.53(2) . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C34A C39A 1.53(2) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C35A C36A 1.50(2) . ?
C35A C40A 1.57(3) . ?
C35A H35A 1.0000 . ?
C36A C37A 1.55(3) . ?
C36A H36C 0.9900 . ?
C36A H36D 0.9900 . ?
C37A C38A 1.51(3) . ?
C37A H37A 1.0000 . ?
C38A C39A 1.51(3) . ?
C38A H38C 0.9900 . ?
C38A H38D 0.9900 . ?
C39A C40A 1.53(2) . ?
C39A H39A 1.0000 . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
N3A C41A 1.454(14) . ?
C41A C43A 1.51(2) . ?
C41A C42A 1.56(2) . ?
C41A C44A 1.558(18) . ?
C42A C45A 1.521(19) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C43A C47A 1.54(2) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C44A C49A 1.547(18) . ?
C44A H44C 0.9900 . ?
C44A H44D 0.9900 . ?
C45A C46A 1.48(3) . ?
C45A C50A 1.58(3) . ?
C45A H45A 1.0000 . ?
C46A C47A 1.56(2) . ?
C46A H46C 0.9900 . ?
C46A H46D 0.9900 . ?
C47A C48A 1.51(3) . ?
C47A H47A 1.0000 . ?
C48A C49A 1.53(2) . ?
C48A H48C 0.9900 . ?
C48A H48D 0.9900 . ?
C49A C50A 1.53(2) . ?
C49A H49A 1.0000 . ?
C50A H50C 0.9900 . ?
C50A H50D 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N2 128.3(17) . . ?
N3A Ni1 N2A 136.9(10) . . ?
N3 Ni1 N1 140.4(15) . . ?
N2 Ni1 N1 90.7(18) . . ?
N3A Ni1 N1A 128.9(11) . . ?
N2A Ni1 N1A 92.7(9) . . ?
C2 C1 C6 121(3) . . ?
C2 C1 C11 114(4) . . ?
C6 C1 C11 125(4) . . ?
C5 N1 C2 107(2) . . ?
C5 N1 Ni1 128(3) . . ?
C2 N1 Ni1 124(3) . . ?
C1 C2 C3 131(4) . . ?
C1 C2 N1 120(3) . . ?
C3 C2 N1 106(2) . . ?
C4 C3 C2 110(3) . . ?
C4 C3 H3 125.0 . . ?
C2 C3 H3 125.0 . . ?
C3 C4 C5 106(3) . . ?
C3 C4 H4 127.1 . . ?
C5 C4 H4 127.1 . . ?
N1 C5 C4 111(3) . . ?
N1 C5 C21 125(3) . . ?
C4 C5 C21 124(3) . . ?
C9 N2 C6 109(2) . . ?
C9 N2 Ni1 133(2) . . ?
C6 N2 Ni1 117.8(17) . . ?
C1 C6 N2 131(2) . . ?
C1 C6 C7 124(3) . . ?
N2 C6 C7 105(2) . . ?
C8 C7 C6 105(2) . . ?
C8 C7 H7 127.4 . . ?
C6 C7 H7 127.4 . . ?
C9 C8 C7 107(2) . . ?
C9 C8 H8 126.4 . . ?
C7 C8 H8 126.4 . . ?
N2 C9 C8 108(3) . . ?
N2 C9 C31 123(3) . . ?
C8 C9 C31 126(3) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C1 114(3) . . ?
C16 C11 C1 124(3) . . ?
F1 C12 C11 118.0(13) . . ?
F1 C12 C13 117.9(16) . . ?
C11 C12 C13 120.0 . . ?
F2 C13 C14 123(5) . . ?
F2 C13 C12 116(5) . . ?
C14 C13 C12 120.0 . . ?
F3 C14 C13 116(2) . . ?
F3 C14 C15 123(2) . . ?
C13 C14 C15 120.0 . . ?
F4 C15 C16 125(2) . . ?
F4 C15 C14 114(2) . . ?
C16 C15 C14 120.0 . . ?
F5 C16 C15 117(3) . . ?
F5 C16 C11 123(3) . . ?
C15 C16 C11 120.0 . . ?
C5 C21 C23 115(3) . . ?
C5 C21 C22 107(3) . . ?
C23 C21 C22 111(2) . . ?
C5 C21 C24 107(3) . . ?
C23 C21 C24 109(2) . . ?
C22 C21 C24 108(2) . . ?
C25 C22 C21 109.3(19) . . ?
C25 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
C25 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
C21 C23 C27 110(2) . . ?
C21 C23 H23A 109.7 . . ?
C27 C23 H23A 109.7 . . ?
C21 C23 H23B 109.7 . . ?
C27 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C29 C24 C21 110(2) . . ?
C29 C24 H24A 109.7 . . ?
C21 C24 H24A 109.7 . . ?
C29 C24 H24B 109.7 . . ?
C21 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C26 C25 C22 110(2) . . ?
C26 C25 C30 109(2) . . ?
C22 C25 C30 107(2) . . ?
C26 C25 H25 110.5 . . ?
C22 C25 H25 110.5 . . ?
C30 C25 H25 110.5 . . ?
C25 C26 C27 111(2) . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C23 110(2) . . ?
C28 C27 C26 110(2) . . ?
C23 C27 C26 107(2) . . ?
C28 C27 H27 109.9 . . ?
C23 C27 H27 109.9 . . ?
C26 C27 H27 109.9 . . ?
C27 C28 C29 111(2) . . ?
C27 C28 H28A 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C29 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C24 108(2) . . ?
C30 C29 C28 108(2) . . ?
C24 C29 C28 110(2) . . ?
C30 C29 H29 110.2 . . ?
C24 C29 H29 110.2 . . ?
C28 C29 H29 110.2 . . ?
C29 C30 C25 112(2) . . ?
C29 C30 H30A 109.2 . . ?
C25 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
C25 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C9 C31 C33 110(3) . . ?
C9 C31 C34 110(3) . . ?
C33 C31 C34 110(2) . . ?
C9 C31 C32 109(3) . . ?
C33 C31 C32 109(2) . . ?
C34 C31 C32 109(2) . . ?
C35 C32 C31 109(2) . . ?
C35 C32 H32A 109.9 . . ?
C31 C32 H32A 109.9 . . ?
C35 C32 H32B 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C31 C33 C37 111(2) . . ?
C31 C33 H33A 109.5 . . ?
C37 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C37 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C39 C34 C31 109(2) . . ?
C39 C34 H34A 109.9 . . ?
C31 C34 H34A 109.9 . . ?
C39 C34 H34B 109.9 . . ?
C31 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C36 C35 C32 112(3) . . ?
C36 C35 C40 108(2) . . ?
C32 C35 C40 108(2) . . ?
C36 C35 H35 109.6 . . ?
C32 C35 H35 109.6 . . ?
C40 C35 H35 109.6 . . ?
C35 C36 C37 109(2) . . ?
C35 C36 H36A 109.9 . . ?
C37 C36 H36A 109.9 . . ?
C35 C36 H36B 109.9 . . ?
C37 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
C38 C37 C33 109(3) . . ?
C38 C37 C36 112(3) . . ?
C33 C37 C36 107(2) . . ?
C38 C37 H37 109.9 . . ?
C33 C37 H37 109.9 . . ?
C36 C37 H37 109.9 . . ?
C37 C38 C39 111(2) . . ?
C37 C38 H38A 109.4 . . ?
C39 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
C39 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C40 C39 C38 109(2) . . ?
C40 C39 C34 108(2) . . ?
C38 C39 C34 110(2) . . ?
C40 C39 H39 110.1 . . ?
C38 C39 H39 110.1 . . ?
C34 C39 H39 110.1 . . ?
C39 C40 C35 112(2) . . ?
C39 C40 H40A 109.2 . . ?
C35 C40 H40A 109.2 . . ?
C39 C40 H40B 109.2 . . ?
C35 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C41 N3 Ni1 164.8(17) . . ?
N3 C41 C43 108(2) . . ?
N3 C41 C44 109(2) . . ?
C43 C41 C44 110(2) . . ?
N3 C41 C42 112(3) . . ?
C43 C41 C42 110(2) . . ?
C44 C41 C42 108(2) . . ?
C45 C42 C41 111(2) . . ?
C45 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
C45 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C41 C43 C47 108(2) . . ?
C41 C43 H43A 110.0 . . ?
C47 C43 H43A 110.0 . . ?
C41 C43 H43B 110.0 . . ?
C47 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
C49 C44 C41 110.2(19) . . ?
C49 C44 H44A 109.6 . . ?
C41 C44 H44A 109.6 . . ?
C49 C44 H44B 109.6 . . ?
C41 C44 H44B 109.6 . . ?
H44A C44 H44B 108.1 . . ?
C46 C45 C42 110(3) . . ?
C46 C45 C50 107(2) . . ?
C42 C45 C50 108(3) . . ?
C46 C45 H45 110.7 . . ?
C42 C45 H45 110.7 . . ?
C50 C45 H45 110.7 . . ?
C45 C46 C47 111(2) . . ?
C45 C46 H46A 109.4 . . ?
C47 C46 H46A 109.4 . . ?
C45 C46 H46B 109.4 . . ?
C47 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
C48 C47 C43 109(3) . . ?
C48 C47 C46 110(3) . . ?
C43 C47 C46 109(2) . . ?
C48 C47 H47 109.5 . . ?
C43 C47 H47 109.5 . . ?
C46 C47 H47 109.5 . . ?
C47 C48 C49 111(2) . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C50 C49 C48 109(2) . . ?
C50 C49 C44 110(3) . . ?
C48 C49 C44 108(2) . . ?
C50 C49 H49 110.2 . . ?
C48 C49 H49 110.2 . . ?
C44 C49 H49 110.2 . . ?
C49 C50 C45 111(2) . . ?
C49 C50 H50A 109.4 . . ?
C45 C50 H50A 109.4 . . ?
C49 C50 H50B 109.4 . . ?
C45 C50 H50B 109.4 . . ?
H50A C50 H50B 108.0 . . ?
C2A C1A C6A 128.5(19) . . ?
C2A C1A C11A 108(3) . . ?
C6A C1A C11A 121(3) . . ?
C5A N1A C2A 105.3(19) . . ?
C5A N1A Ni1 133.9(19) . . ?
C2A N1A Ni1 119.3(16) . . ?
C1A C2A C3A 130(2) . . ?
C1A C2A N1A 120(2) . . ?
C3A C2A N1A 108(2) . . ?
C4A C3A C2A 108(2) . . ?
C4A C3A H3A 125.8 . . ?
C2A C3A H3A 125.8 . . ?
C3A C4A C5A 107(2) . . ?
C3A C4A H4A 126.5 . . ?
C5A C4A H4A 126.5 . . ?
N1A C5A C4A 111(2) . . ?
N1A C5A C21A 123(2) . . ?
C4A C5A C21A 126(2) . . ?
C9A N2A C6A 107.8(17) . . ?
C9A N2A Ni1 131.2(17) . . ?
C6A N2A Ni1 117.3(15) . . ?
C1A C6A N2A 122.7(17) . . ?
C1A C6A C7A 127(2) . . ?
N2A C6A C7A 108.4(17) . . ?
C8A C7A C6A 105(2) . . ?
C8A C7A H7A 127.3 . . ?
C6A C7A H7A 127.3 . . ?
C9A C8A C7A 108.6(19) . . ?
C9A C8A H8A 125.7 . . ?
C7A C8A H8A 125.7 . . ?
N2A C9A C8A 109(2) . . ?
N2A C9A C31A 120(2) . . ?
C8A C9A C31A 131(2) . . ?
C16A C11A C12A 115.4(15) . . ?
C16A C11A C1A 119(2) . . ?
C12A C11A C1A 125(2) . . ?
F1A C12A C11A 119.0(17) . . ?
F1A C12A C13A 117.3(14) . . ?
C11A C12A C13A 120.5(17) . . ?
F2A C13A C14A 115(3) . . ?
F2A C13A C12A 123(3) . . ?
C14A C13A C12A 121.2(14) . . ?
C15A C14A F3A 116.1(19) . . ?
C15A C14A C13A 119.4(15) . . ?
F3A C14A C13A 122.5(18) . . ?
C14A C15A F4A 122.9(19) . . ?
C14A C15A C16A 117.3(18) . . ?
F4A C15A C16A 119(2) . . ?
C11A C16A F5A 120(2) . . ?
C11A C16A C15A 125.3(16) . . ?
F5A C16A C15A 115(2) . . ?
C5A C21A C23A 108.8(19) . . ?
C5A C21A C22A 111.6(19) . . ?
C23A C21A C22A 109.1(18) . . ?
C5A C21A C24A 111.0(17) . . ?
C23A C21A C24A 106.7(16) . . ?
C22A C21A C24A 109.6(16) . . ?
C25A C22A C21A 112.3(16) . . ?
C25A C22A H22C 109.1 . . ?
C21A C22A H22C 109.1 . . ?
C25A C22A H22D 109.1 . . ?
C21A C22A H22D 109.1 . . ?
H22C C22A H22D 107.9 . . ?
C21A C23A C27A 112.4(16) . . ?
C21A C23A H23C 109.1 . . ?
C27A C23A H23C 109.1 . . ?
C21A C23A H23D 109.1 . . ?
C27A C23A H23D 109.1 . . ?
H23C C23A H23D 107.9 . . ?
C29A C24A C21A 108.2(15) . . ?
C29A C24A H24C 110.0 . . ?
C21A C24A H24C 110.0 . . ?
C29A C24A H24D 110.0 . . ?
C21A C24A H24D 110.0 . . ?
H24C C24A H24D 108.4 . . ?
C26A C25A C22A 110.1(18) . . ?
C26A C25A C30A 108.5(17) . . ?
C22A C25A C30A 105.4(18) . . ?
C26A C25A H25A 110.9 . . ?
C22A C25A H25A 110.9 . . ?
C30A C25A H25A 110.9 . . ?
C25A C26A C27A 110.4(17) . . ?
C25A C26A H26C 109.6 . . ?
C27A C26A H26C 109.6 . . ?
C25A C26A H26D 109.6 . . ?
C27A C26A H26D 109.6 . . ?
H26C C26A H26D 108.1 . . ?
C28A C27A C23A 109.5(18) . . ?
C28A C27A C26A 108.7(18) . . ?
C23A C27A C26A 108.1(18) . . ?
C28A C27A H27A 110.1 . . ?
C23A C27A H27A 110.1 . . ?
C26A C27A H27A 110.1 . . ?
C27A C28A C29A 109.9(17) . . ?
C27A C28A H28C 109.7 . . ?
C29A C28A H28C 109.7 . . ?
C27A C28A H28D 109.7 . . ?
C29A C28A H28D 109.7 . . ?
H28C C28A H28D 108.2 . . ?
C30A C29A C24A 111.8(17) . . ?
C30A C29A C28A 106.2(17) . . ?
C24A C29A C28A 111.6(17) . . ?
C30A C29A H29A 109.0 . . ?
C24A C29A H29A 109.0 . . ?
C28A C29A H29A 109.0 . . ?
C29A C30A C25A 111.3(15) . . ?
C29A C30A H30C 109.4 . . ?
C25A C30A H30C 109.4 . . ?
C29A C30A H30D 109.4 . . ?
C25A C30A H30D 109.4 . . ?
H30C C30A H30D 108.0 . . ?
C9A C31A C33A 110.0(18) . . ?
C9A C31A C32A 110.6(18) . . ?
C33A C31A C32A 109.2(17) . . ?
C9A C31A C34A 111.1(16) . . ?
C33A C31A C34A 107.8(16) . . ?
C32A C31A C34A 108.0(18) . . ?
C35A C32A C31A 110.3(16) . . ?
C35A C32A H32C 109.6 . . ?
C31A C32A H32C 109.6 . . ?
C35A C32A H32D 109.6 . . ?
C31A C32A H32D 109.6 . . ?
H32C C32A H32D 108.1 . . ?
C31A C33A C37A 110.7(18) . . ?
C31A C33A H33C 109.5 . . ?
C37A C33A H33C 109.5 . . ?
C31A C33A H33D 109.5 . . ?
C37A C33A H33D 109.5 . . ?
H33C C33A H33D 108.1 . . ?
C39A C34A C31A 111.1(16) . . ?
C39A C34A H34C 109.4 . . ?
C31A C34A H34C 109.4 . . ?
C39A C34A H34D 109.4 . . ?
C31A C34A H34D 109.4 . . ?
H34C C34A H34D 108.0 . . ?
C36A C35A C32A 110(2) . . ?
C36A C35A C40A 110.4(18) . . ?
C32A C35A C40A 108.5(19) . . ?
C36A C35A H35A 109.3 . . ?
C32A C35A H35A 109.3 . . ?
C40A C35A H35A 109.3 . . ?
C35A C36A C37A 109.6(18) . . ?
C35A C36A H36C 109.7 . . ?
C37A C36A H36C 109.7 . . ?
C35A C36A H36D 109.7 . . ?
C37A C36A H36D 109.8 . . ?
H36C C36A H36D 108.2 . . ?
C38A C37A C33A 109(2) . . ?
C38A C37A C36A 109(2) . . ?
C33A C37A C36A 109(2) . . ?
C38A C37A H37A 109.9 . . ?
C33A C37A H37A 109.9 . . ?
C36A C37A H37A 109.9 . . ?
C39A C38A C37A 111.5(19) . . ?
C39A C38A H38C 109.3 . . ?
C37A C38A H38C 109.3 . . ?
C39A C38A H38D 109.3 . . ?
C37A C38A H38D 109.3 . . ?
H38C C38A H38D 108.0 . . ?
C38A C39A C34A 107.7(19) . . ?
C38A C39A C40A 110.6(19) . . ?
C34A C39A C40A 109.0(18) . . ?
C38A C39A H39A 109.8 . . ?
C34A C39A H39A 109.8 . . ?
C40A C39A H39A 109.8 . . ?
C39A C40A C35A 108.8(18) . . ?
C39A C40A H40C 109.9 . . ?
C35A C40A H40C 109.9 . . ?
C39A C40A H40D 109.9 . . ?
C35A C40A H40D 109.9 . . ?
H40C C40A H40D 108.3 . . ?
C41A N3A Ni1 163.4(11) . . ?
N3A C41A C43A 106.5(18) . . ?
N3A C41A C42A 111.3(15) . . ?
C43A C41A C42A 109.7(16) . . ?
N3A C41A C44A 111.3(15) . . ?
C43A C41A C44A 109.8(17) . . ?
C42A C41A C44A 108.2(17) . . ?
C45A C42A C41A 111.4(15) . . ?
C45A C42A H42C 109.3 . . ?
C41A C42A H42C 109.3 . . ?
C45A C42A H42D 109.3 . . ?
C41A C42A H42D 109.3 . . ?
H42C C42A H42D 108.0 . . ?
C41A C43A C47A 109.5(16) . . ?
C41A C43A H43C 109.8 . . ?
C47A C43A H43C 109.8 . . ?
C41A C43A H43D 109.8 . . ?
C47A C43A H43D 109.8 . . ?
H43C C43A H43D 108.2 . . ?
C49A C44A C41A 109.1(14) . . ?
C49A C44A H44C 109.9 . . ?
C41A C44A H44C 109.9 . . ?
C49A C44A H44D 109.9 . . ?
C41A C44A H44D 109.9 . . ?
H44C C44A H44D 108.3 . . ?
C46A C45A C42A 109.1(19) . . ?
C46A C45A C50A 108.5(18) . . ?
C42A C45A C50A 107.1(17) . . ?
C46A C45A H45A 110.7 . . ?
C42A C45A H45A 110.7 . . ?
C50A C45A H45A 110.7 . . ?
C45A C46A C47A 113.0(16) . . ?
C45A C46A H46C 109.0 . . ?
C47A C46A H46C 109.0 . . ?
C45A C46A H46D 109.0 . . ?
C47A C46A H46D 109.0 . . ?
H46C C46A H46D 107.8 . . ?
C48A C47A C43A 109.0(18) . . ?
C48A C47A C46A 107.4(18) . . ?
C43A C47A C46A 109.3(18) . . ?
C48A C47A H47A 110.3 . . ?
C43A C47A H47A 110.3 . . ?
C46A C47A H47A 110.3 . . ?
C47A C48A C49A 111.4(18) . . ?
C47A C48A H48C 109.3 . . ?
C49A C48A H48C 109.3 . . ?
C47A C48A H48D 109.3 . . ?
C49A C48A H48D 109.3 . . ?
H48C C48A H48D 108.0 . . ?
C48A C49A C50A 111.7(18) . . ?
C48A C49A C44A 107.5(18) . . ?
C50A C49A C44A 108.6(18) . . ?
C48A C49A H49A 109.6 . . ?
C50A C49A H49A 109.6 . . ?
C44A C49A H49A 109.6 . . ?
C49A C50A C45A 109.7(17) . . ?
C49A C50A H50C 109.7 . . ?
C45A C50A H50C 109.7 . . ?
C49A C50A H50D 109.7 . . ?
C45A C50A H50D 109.7 . . ?
H50C C50A H50D 108.2 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 157(5) . . . . ?
C11 C1 C2 C3 -27(9) . . . . ?
C6 C1 C2 N1 -4(8) . . . . ?
C11 C1 C2 N1 172(4) . . . . ?
C5 N1 C2 C1 164(5) . . . . ?
Ni1 N1 C2 C1 -30(7) . . . . ?
C5 N1 C2 C3 -1(6) . . . . ?
Ni1 N1 C2 C3 165(4) . . . . ?
C1 C2 C3 C4 -158(6) . . . . ?
N1 C2 C3 C4 5(6) . . . . ?
C2 C3 C4 C5 -7(6) . . . . ?
C2 N1 C5 C4 -3(6) . . . . ?
Ni1 N1 C5 C4 -169(4) . . . . ?
C2 N1 C5 C21 -175(4) . . . . ?
Ni1 N1 C5 C21 19(7) . . . . ?
C3 C4 C5 N1 7(6) . . . . ?
C3 C4 C5 C21 179(4) . . . . ?
N3 Ni1 N2 C9 -34(7) . . . . ?
N1 Ni1 N2 C9 154(6) . . . . ?
N3 Ni1 N2 C6 139(3) . . . . ?
N1 Ni1 N2 C6 -33(4) . . . . ?
C2 C1 C6 N2 12(8) . . . . ?
C11 C1 C6 N2 -163(5) . . . . ?
C2 C1 C6 C7 -176(5) . . . . ?
C11 C1 C6 C7 9(7) . . . . ?
C9 N2 C6 C1 -171(4) . . . . ?
Ni1 N2 C6 C1 14(7) . . . . ?
C9 N2 C6 C7 16(5) . . . . ?
Ni1 N2 C6 C7 -159(4) . . . . ?
C1 C6 C7 C8 164(4) . . . . ?
N2 C6 C7 C8 -22(5) . . . . ?
C6 C7 C8 C9 20(5) . . . . ?
C6 N2 C9 C8 -3(6) . . . . ?
Ni1 N2 C9 C8 170(5) . . . . ?
C6 N2 C9 C31 157(4) . . . . ?
Ni1 N2 C9 C31 -29(9) . . . . ?
C7 C8 C9 N2 -11(6) . . . . ?
C7 C8 C9 C31 -171(4) . . . . ?
C2 C1 C11 C12 84(5) . . . . ?
C6 C1 C11 C12 -101(5) . . . . ?
C2 C1 C11 C16 -111(5) . . . . ?
C6 C1 C11 C16 65(7) . . . . ?
C16 C11 C12 F1 -157(4) . . . . ?
C1 C11 C12 F1 10(3) . . . . ?
C16 C11 C12 C13 0.0 . . . . ?
C1 C11 C12 C13 166(6) . . . . ?
F1 C12 C13 F2 -8(6) . . . . ?
C11 C12 C13 F2 -165(5) . . . . ?
F1 C12 C13 C14 157(4) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
F2 C13 C14 F3 -6(6) . . . . ?
C12 C13 C14 F3 -170(5) . . . . ?
F2 C13 C14 C15 164(5) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
F3 C14 C15 F4 -6(4) . . . . ?
C13 C14 C15 F4 -176(4) . . . . ?
F3 C14 C15 C16 169(5) . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
F4 C15 C16 F5 -2(6) . . . . ?
C14 C15 C16 F5 -178(5) . . . . ?
F4 C15 C16 C11 175(4) . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
C12 C11 C16 F5 178(5) . . . . ?
C1 C11 C16 F5 13(5) . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
C1 C11 C16 C15 -165(7) . . . . ?
N1 C5 C21 C23 34(6) . . . . ?
C4 C5 C21 C23 -137(4) . . . . ?
N1 C5 C21 C22 -89(5) . . . . ?
C4 C5 C21 C22 100(5) . . . . ?
N1 C5 C21 C24 155(4) . . . . ?
C4 C5 C21 C24 -16(5) . . . . ?
C5 C21 C22 C25 -177(3) . . . . ?
C23 C21 C22 C25 57(3) . . . . ?
C24 C21 C22 C25 -63(3) . . . . ?
C5 C21 C23 C27 179(3) . . . . ?
C22 C21 C23 C27 -59(3) . . . . ?
C24 C21 C23 C27 60(3) . . . . ?
C5 C21 C24 C29 176(3) . . . . ?
C23 C21 C24 C29 -59(3) . . . . ?
C22 C21 C24 C29 62(3) . . . . ?
C21 C22 C25 C26 -57(3) . . . . ?
C21 C22 C25 C30 61(3) . . . . ?
C22 C25 C26 C27 61(3) . . . . ?
C30 C25 C26 C27 -55(3) . . . . ?
C21 C23 C27 C28 -60(3) . . . . ?
C21 C23 C27 C26 60(3) . . . . ?
C25 C26 C27 C28 58(3) . . . . ?
C25 C26 C27 C23 -62(3) . . . . ?
C23 C27 C28 C29 58(3) . . . . ?
C26 C27 C28 C29 -60(3) . . . . ?
C21 C24 C29 C30 -60(3) . . . . ?
C21 C24 C29 C28 58(3) . . . . ?
C27 C28 C29 C30 61(3) . . . . ?
C27 C28 C29 C24 -57(3) . . . . ?
C24 C29 C30 C25 60(3) . . . . ?
C28 C29 C30 C25 -59(3) . . . . ?
C26 C25 C30 C29 58(3) . . . . ?
C22 C25 C30 C29 -60(3) . . . . ?
N2 C9 C31 C33 -164(5) . . . . ?
C8 C9 C31 C33 -8(6) . . . . ?
N2 C9 C31 C34 -43(6) . . . . ?
C8 C9 C31 C34 114(5) . . . . ?
N2 C9 C31 C32 76(5) . . . . ?
C8 C9 C31 C32 -127(5) . . . . ?
C9 C31 C32 C35 177(3) . . . . ?
C33 C31 C32 C35 57(3) . . . . ?
C34 C31 C32 C35 -63(3) . . . . ?
C9 C31 C33 C37 179(3) . . . . ?
C34 C31 C33 C37 58(3) . . . . ?
C32 C31 C33 C37 -62(3) . . . . ?
C9 C31 C34 C39 -179(3) . . . . ?
C33 C31 C34 C39 -57(3) . . . . ?
C32 C31 C34 C39 62(3) . . . . ?
C31 C32 C35 C36 -59(3) . . . . ?
C31 C32 C35 C40 60(3) . . . . ?
C32 C35 C36 C37 60(3) . . . . ?
C40 C35 C36 C37 -58(3) . . . . ?
C31 C33 C37 C38 -58(4) . . . . ?
C31 C33 C37 C36 62(3) . . . . ?
C35 C36 C37 C38 59(3) . . . . ?
C35 C36 C37 C33 -60(3) . . . . ?
C33 C37 C38 C39 60(3) . . . . ?
C36 C37 C38 C39 -57(3) . . . . ?
C37 C38 C39 C40 57(3) . . . . ?
C37 C38 C39 C34 -61(3) . . . . ?
C31 C34 C39 C40 -60(3) . . . . ?
C31 C34 C39 C38 58(3) . . . . ?
C38 C39 C40 C35 -59(3) . . . . ?
C34 C39 C40 C35 60(3) . . . . ?
C36 C35 C40 C39 61(3) . . . . ?
C32 C35 C40 C39 -61(3) . . . . ?
N2 Ni1 N3 C41 -103(8) . . . . ?
N1 Ni1 N3 C41 65(9) . . . . ?
Ni1 N3 C41 C43 61(9) . . . . ?
Ni1 N3 C41 C44 -179(7) . . . . ?
Ni1 N3 C41 C42 -60(9) . . . . ?
N3 C41 C42 C45 178(3) . . . . ?
C43 C41 C42 C45 59(3) . . . . ?
C44 C41 C42 C45 -61(3) . . . . ?
N3 C41 C43 C47 179(3) . . . . ?
C44 C41 C43 C47 59(3) . . . . ?
C42 C41 C43 C47 -59(3) . . . . ?
N3 C41 C44 C49 -178(3) . . . . ?
C43 C41 C44 C49 -59(3) . . . . ?
C42 C41 C44 C49 60(3) . . . . ?
C41 C42 C45 C46 -57(4) . . . . ?
C41 C42 C45 C50 59(3) . . . . ?
C42 C45 C46 C47 58(3) . . . . ?
C50 C45 C46 C47 -59(3) . . . . ?
C41 C43 C47 C48 -60(3) . . . . ?
C41 C43 C47 C46 60(3) . . . . ?
C45 C46 C47 C48 60(3) . . . . ?
C45 C46 C47 C43 -60(3) . . . . ?
C43 C47 C48 C49 62(3) . . . . ?
C46 C47 C48 C49 -57(3) . . . . ?
C47 C48 C49 C50 58(3) . . . . ?
C47 C48 C49 C44 -61(3) . . . . ?
C41 C44 C49 C50 -60(3) . . . . ?
C41 C44 C49 C48 58(4) . . . . ?
C48 C49 C50 C45 -59(3) . . . . ?
C44 C49 C50 C45 58(3) . . . . ?
C46 C45 C50 C49 60(3) . . . . ?
C42 C45 C50 C49 -58(3) . . . . ?
C6A C1A C2A C3A 158(3) . . . . ?
C11A C1A C2A C3A -6(5) . . . . ?
C6A C1A C2A N1A -5(5) . . . . ?
C11A C1A C2A N1A -169(2) . . . . ?
C5A N1A C2A C1A 167(3) . . . . ?
Ni1 N1A C2A C1A -25(4) . . . . ?
C5A N1A C2A C3A 1(3) . . . . ?
Ni1 N1A C2A C3A 169(2) . . . . ?
C1A C2A C3A C4A -168(3) . . . . ?
N1A C2A C3A C4A -4(4) . . . . ?
C2A C3A C4A C5A 4(4) . . . . ?
C2A N1A C5A C4A 1(3) . . . . ?
Ni1 N1A C5A C4A -164(2) . . . . ?
C2A N1A C5A C21A -174(3) . . . . ?
Ni1 N1A C5A C21A 21(5) . . . . ?
C3A C4A C5A N1A -4(4) . . . . ?
C3A C4A C5A C21A 171(3) . . . . ?
C2A C1A C6A N2A 3(5) . . . . ?
C11A C1A C6A N2A 165(3) . . . . ?
C2A C1A C6A C7A -158(3) . . . . ?
C11A C1A C6A C7A 4(4) . . . . ?
C9A N2A C6A C1A -171(2) . . . . ?
Ni1 N2A C6A C1A 28(3) . . . . ?
C9A N2A C6A C7A -7(3) . . . . ?
Ni1 N2A C6A C7A -167.6(16) . . . . ?
C1A C6A C7A C8A 168(3) . . . . ?
N2A C6A C7A C8A 5(3) . . . . ?
C6A C7A C8A C9A -2(3) . . . . ?
C6A N2A C9A C8A 6(3) . . . . ?
Ni1 N2A C9A C8A 163(2) . . . . ?
C6A N2A C9A C31A -178(2) . . . . ?
Ni1 N2A C9A C31A -20(4) . . . . ?
C7A C8A C9A N2A -2(3) . . . . ?
C7A C8A C9A C31A -179(2) . . . . ?
C2A C1A C11A C16A -85(5) . . . . ?
C6A C1A C11A C16A 110(5) . . . . ?
C2A C1A C11A C12A 105(5) . . . . ?
C6A C1A C11A C12A -60(6) . . . . ?
C16A C11A C12A F1A 169(5) . . . . ?
C1A C11A C12A F1A -21(6) . . . . ?
C16A C11A C12A C13A 9(6) . . . . ?
C1A C11A C12A C13A 180(5) . . . . ?
F1A C12A C13A F2A 4(6) . . . . ?
C11A C12A C13A F2A 164(4) . . . . ?
F1A C12A C13A C14A -163(2) . . . . ?
C11A C12A C13A C14A -4(5) . . . . ?
F2A C13A C14A C15A -174(4) . . . . ?
C12A C13A C14A C15A -5(5) . . . . ?
F2A C13A C14A F3A 23(5) . . . . ?
C12A C13A C14A F3A -168(3) . . . . ?
F3A C14A C15A F4A 0(4) . . . . ?
C13A C14A C15A F4A -164(3) . . . . ?
F3A C14A C15A C16A 172(3) . . . . ?
C13A C14A C15A C16A 7(4) . . . . ?
C12A C11A C16A F5A 170(4) . . . . ?
C1A C11A C16A F5A -1(7) . . . . ?
C12A C11A C16A C15A -7(7) . . . . ?
C1A C11A C16A C15A -178(4) . . . . ?
C14A C15A C16A C11A -1(6) . . . . ?
F4A C15A C16A C11A 170(4) . . . . ?
C14A C15A C16A F5A -179(3) . . . . ?
F4A C15A C16A F5A -7(5) . . . . ?
N1A C5A C21A C23A 50(3) . . . . ?
C4A C5A C21A C23A -124(3) . . . . ?
N1A C5A C21A C22A -70(3) . . . . ?
C4A C5A C21A C22A 116(3) . . . . ?
N1A C5A C21A C24A 168(3) . . . . ?
C4A C5A C21A C24A -7(4) . . . . ?
C5A C21A C22A C25A 175(2) . . . . ?
C23A C21A C22A C25A 55(2) . . . . ?
C24A C21A C22A C25A -62(2) . . . . ?
C5A C21A C23A C27A -179(2) . . . . ?
C22A C21A C23A C27A -57(2) . . . . ?
C24A C21A C23A C27A 62(2) . . . . ?
C5A C21A C24A C29A -179(2) . . . . ?
C23A C21A C24A C29A -61(2) . . . . ?
C22A C21A C24A C29A 57(2) . . . . ?
C21A C22A C25A C26A -57(2) . . . . ?
C21A C22A C25A C30A 60(2) . . . . ?
C22A C25A C26A C27A 59(3) . . . . ?
C30A C25A C26A C27A -56(2) . . . . ?
C21A C23A C27A C28A -60(2) . . . . ?
C21A C23A C27A C26A 59(2) . . . . ?
C25A C26A C27A C28A 59(2) . . . . ?
C25A C26A C27A C23A -59(2) . . . . ?
C23A C27A C28A C29A 55(2) . . . . ?
C26A C27A C28A C29A -63(2) . . . . ?
C21A C24A C29A C30A -58(2) . . . . ?
C21A C24A C29A C28A 61(2) . . . . ?
C27A C28A C29A C30A 64(2) . . . . ?
C27A C28A C29A C24A -58(2) . . . . ?
C24A C29A C30A C25A 60(2) . . . . ?
C28A C29A C30A C25A -62(2) . . . . ?
C26A C25A C30A C29A 59(2) . . . . ?
C22A C25A C30A C29A -59(2) . . . . ?
N2A C9A C31A C33A -155(2) . . . . ?
C8A C9A C31A C33A 20(3) . . . . ?
N2A C9A C31A C32A 84(3) . . . . ?
C8A C9A C31A C32A -100(3) . . . . ?
N2A C9A C31A C34A -36(3) . . . . ?
C8A C9A C31A C34A 140(3) . . . . ?
C9A C31A C32A C35A 179(2) . . . . ?
C33A C31A C32A C35A 58(3) . . . . ?
C34A C31A C32A C35A -59(2) . . . . ?
C9A C31A C33A C37A 180(2) . . . . ?
C32A C31A C33A C37A -59(2) . . . . ?
C34A C31A C33A C37A 58(2) . . . . ?
C9A C31A C34A C39A 179.8(19) . . . . ?
C33A C31A C34A C39A -60(2) . . . . ?
C32A C31A C34A C39A 58(2) . . . . ?
C31A C32A C35A C36A -59(3) . . . . ?
C31A C32A C35A C40A 62(2) . . . . ?
C32A C35A C36A C37A 60(3) . . . . ?
C40A C35A C36A C37A -59(2) . . . . ?
C31A C33A C37A C38A -59(3) . . . . ?
C31A C33A C37A C36A 60(2) . . . . ?
C35A C36A C37A C38A 59(3) . . . . ?
C35A C36A C37A C33A -60(3) . . . . ?
C33A C37A C38A C39A 60(3) . . . . ?
C36A C37A C38A C39A -59(3) . . . . ?
C37A C38A C39A C34A -60(3) . . . . ?
C37A C38A C39A C40A 59(3) . . . . ?
C31A C34A C39A C38A 60(2) . . . . ?
C31A C34A C39A C40A -60(2) . . . . ?
C38A C39A C40A C35A -57(2) . . . . ?
C34A C39A C40A C35A 61(2) . . . . ?
C36A C35A C40A C39A 59(2) . . . . ?
C32A C35A C40A C39A -62(2) . . . . ?
N2A Ni1 N3A C41A -107(6) . . . . ?
N1A Ni1 N3A C41A 56(7) . . . . ?
Ni1 N3A C41A C43A 99(6) . . . . ?
Ni1 N3A C41A C42A -21(7) . . . . ?
Ni1 N3A C41A C44A -141(6) . . . . ?
N3A C41A C42A C45A 177(2) . . . . ?
C43A C41A C42A C45A 59(2) . . . . ?
C44A C41A C42A C45A -60(2) . . . . ?
N3A C41A C43A C47A -179.7(17) . . . . ?
C42A C41A C43A C47A -59(2) . . . . ?
C44A C41A C43A C47A 60(2) . . . . ?
N3A C41A C44A C49A -178(2) . . . . ?
C43A C41A C44A C49A -60(2) . . . . ?
C42A C41A C44A C49A 59(2) . . . . ?
C41A C42A C45A C46A -57(2) . . . . ?
C41A C42A C45A C50A 60(2) . . . . ?
C42A C45A C46A C47A 57(2) . . . . ?
C50A C45A C46A C47A -60(2) . . . . ?
C41A C43A C47A C48A -60(2) . . . . ?
C41A C43A C47A C46A 58(2) . . . . ?
C45A C46A C47A C48A 61(2) . . . . ?
C45A C46A C47A C43A -58(2) . . . . ?
C43A C47A C48A C49A 61(2) . . . . ?
C46A C47A C48A C49A -57(2) . . . . ?
C47A C48A C49A C50A 58(2) . . . . ?
C47A C48A C49A C44A -61(2) . . . . ?
C41A C44A C49A C48A 59(2) . . . . ?
C41A C44A C49A C50A -62(2) . . . . ?
C48A C49A C50A C45A -56(2) . . . . ?
C44A C49A C50A C45A 63(2) . . . . ?
C46A C45A C50A C49A 56(2) . . . . ?
C42A C45A C50A C49A -61(2) . . . . ?
_refine_diff_density_max 0.532
_refine_diff_density_min -0.762
_refine_diff_density_rms 0.084
_shelx_res_file
;
4.res created by SHELXL-2014/7
TITL 4.res in Pna2(1)
CELL 1.54178 14.1294 16.6197 15.8282 90 90 90
ZERR 4 0.0009 0.0008 0.0008 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,0.5+Z
SFAC C H F N Ni
UNIT 180 196 20 12 4
SADI C1 C2 C1A C2A C1 C6 C1A C6A
SADI C12 F1 C12A F1A
SADI C13 F2 C13A F2A
SADI C14 F3 C14A F3A
SADI C15 F4 C15A F4A
SADI C16 F5 C16A F5A
SADI C5 C21 C5A C21A
SADI N3 C41 N3A C41A
SADI Ni1 N1 Ni1 N1A
SADI Ni1 N2 Ni1 N2A
SADI Ni1 N3 Ni1 N3A
RIGU Ni1 > C50
EADP N1 N1A
EADP C2 C2A
EADP C3 C3A
EADP C4 C4A
EADP C5 C5A
EADP C6 C6A
EADP C7 C7A
EADP C8 C8A
EADP C9 C9A
EADP N2 N2A
EADP C11 C11A
EADP C12 C12A
EADP C13 C13A
EADP C14 C14A
EADP C15 C15A
EADP C16 C16A
EADP F1 F1A
EADP F2 F2A
EADP F3 F3A
EADP F4 F4A
EADP F5 F5A
EADP C21 C21A
EADP C22 C22A
EADP C23 C23A
EADP C24 C24A
EADP C25 C25A
EADP C26 C26A
EADP C27 C27A
EADP C28 C28A
EADP C29 C29A
EADP C30 C30A
EADP C31 C31A
EADP C32 C32A
EADP C33 C33A
EADP C34 C34A
EADP C35 C35A
EADP C36 C36A
EADP C37 C37A
EADP C38 C38A
EADP C39 C39A
EADP C40 C40A
EADP N3 N3A
EADP C41 C41A
EADP C42 C42A
EADP C43 C43A
EADP C44 C44A
EADP C45 C45A
EADP C46 C46A
EADP C47 C47A
EADP C48 C48A
EADP C49 C49A
EADP C50 C50A
EXYZ N3 N3A
EXYZ C6 C6A
EXYZ C13 C13A
EXYZ F1 F1A
L.S. 100
PLAN -1
SIZE 0.02 0.08 0.12
TEMP -173.15
BOND $H
CONF
LIST 4
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.064700 12.386700
BASF 0.35044
FVAR 0.28582 0.38431 0.33753
NI1 5 -0.613216 -0.730577 -0.525679 11.00000 0.06765 0.03265 =
0.03895 0.00252 0.00644 0.00402
PART 1
C1 1 -0.559196 -0.539044 -0.524683 21.00000 0.03402 0.02607 =
0.05135 -0.00169 0.00617 0.01898
SAME 0.02 0.04 N1A > C5A
N1 4 -0.637572 -0.644917 -0.603172 21.00000 0.07024 0.02828 =
0.04125 0.00092 -0.00121 0.00549
C2 1 -0.590996 -0.569898 -0.600491 21.00000 0.05828 0.02896 =
0.04795 0.00734 -0.00144 0.00915
C3 1 -0.608902 -0.532381 -0.678445 21.00000 0.08788 0.04393 =
0.06450 0.02363 -0.01483 -0.00543
AFIX 43
H3 2 -0.582035 -0.482791 -0.696217 21.00000 -1.20000
AFIX 0
C4 1 -0.669127 -0.576560 -0.723843 21.00000 0.07649 0.05663 =
0.04878 0.02094 -0.00782 -0.00670
AFIX 43
H4 2 -0.697987 -0.562279 -0.775937 21.00000 -1.20000
AFIX 0
C5 1 -0.681094 -0.649110 -0.678294 21.00000 0.06188 0.04237 =
0.04217 0.00399 -0.00034 0.00224
SAME 0.02 0.04 N2A > C9A
N2 4 -0.611778 -0.657221 -0.434421 21.00000 0.02945 0.03365 =
0.03965 -0.00109 -0.00256 0.00848
C6 1 -0.577012 -0.578803 -0.449779 21.00000 0.05362 0.03456 =
0.04857 -0.00804 0.00326 0.00021
C7 1 -0.550727 -0.547574 -0.367301 21.00000 0.03657 0.05483 =
0.05364 -0.01870 0.00134 0.01024
AFIX 43
H7 2 -0.507597 -0.505217 -0.355387 21.00000 -1.20000
AFIX 0
C8 1 -0.603905 -0.594446 -0.307642 21.00000 0.04405 0.07174 =
0.05053 -0.02081 0.00603 -0.00037
AFIX 43
H8 2 -0.618079 -0.579936 -0.250984 21.00000 -1.20000
AFIX 0
C9 1 -0.631083 -0.665839 -0.348748 21.00000 0.02809 0.05968 =
0.04282 -0.00097 0.00350 0.00769
AFIX 66
C11 1 -0.500317 -0.465746 -0.532888 21.00000 0.06039 0.03382 =
0.04833 0.00106 0.00390 -0.00238
C12 1 -0.551721 -0.394717 -0.539514 21.00000 0.06493 0.03546 =
0.03085 0.00377 0.00246 0.00272
C13 1 -0.506570 -0.321018 -0.529557 21.00000 0.07406 0.03062 =
0.07443 0.00079 0.00810 0.00556
C14 1 -0.410015 -0.318348 -0.512975 21.00000 0.07262 0.02868 =
0.05819 0.01001 0.01829 -0.00132
C15 1 -0.358610 -0.389377 -0.506349 21.00000 0.06136 0.03992 =
0.05640 0.01054 0.02512 -0.00327
C16 1 -0.403760 -0.463077 -0.516305 21.00000 0.06440 0.02741 =
0.06837 0.01564 0.00711 0.00352
AFIX 0
F1 3 -0.646103 -0.397925 -0.525334 21.00000 0.07145 0.04287 =
0.05334 0.01374 0.00545 0.00394
F2 3 -0.564857 -0.256440 -0.517278 21.00000 0.08473 0.03372 =
0.04547 0.00254 0.01149 0.00540
F3 3 -0.373454 -0.244756 -0.490788 21.00000 0.08496 0.03577 =
0.07364 -0.00258 0.02989 -0.00925
F4 3 -0.267890 -0.379312 -0.484909 21.00000 0.06336 0.04721 =
0.08028 0.01200 0.02309 -0.00469
F5 3 -0.349962 -0.530621 -0.505974 21.00000 0.06480 0.03493 =
0.07772 0.01207 0.00887 0.00226
SAME 0.02 0.04 C21A > C30A
SAME 0.02 0.04 C31 > C40
SAME 0.02 0.04 C31A > C40A
SAME 0.02 0.04 C41 > C50
SAME 0.02 0.04 C41A > C50A
C21 1 -0.745771 -0.716970 -0.706255 21.00000 0.05934 0.05875 =
0.04309 -0.01297 0.00164 -0.00070
C22 1 -0.681943 -0.780989 -0.748978 21.00000 0.04420 0.05983 =
0.04084 -0.01610 0.00177 -0.00194
AFIX 23
H22A 2 -0.646260 -0.756179 -0.796083 21.00000 -1.20000
H22B 2 -0.635857 -0.802293 -0.707514 21.00000 -1.20000
AFIX 0
C23 1 -0.805238 -0.754218 -0.635950 21.00000 0.06397 0.05294 =
0.05041 -0.01506 0.01058 0.00207
AFIX 23
H23A 2 -0.845208 -0.712254 -0.609540 21.00000 -1.20000
H23B 2 -0.763144 -0.776742 -0.591896 21.00000 -1.20000
AFIX 0
C24 1 -0.813161 -0.681336 -0.774486 21.00000 0.05639 0.08057 =
0.04647 -0.00760 0.00188 -0.00213
AFIX 23
H24A 2 -0.852939 -0.638707 -0.749039 21.00000 -1.20000
H24B 2 -0.775426 -0.656938 -0.820542 21.00000 -1.20000
AFIX 0
C25 1 -0.743875 -0.849737 -0.782645 21.00000 0.04530 0.06941 =
0.07262 -0.02945 -0.00058 -0.00462
AFIX 13
H25 2 -0.703804 -0.892096 -0.809733 21.00000 -1.20000
AFIX 0
C26 1 -0.800767 -0.884923 -0.711617 21.00000 0.04371 0.06405 =
0.07147 -0.03184 0.00354 -0.00902
AFIX 23
H26A 2 -0.757389 -0.905578 -0.667546 21.00000 -1.20000
H26B 2 -0.838532 -0.930744 -0.733083 21.00000 -1.20000
AFIX 0
C27 1 -0.868297 -0.821160 -0.671986 21.00000 0.05327 0.06254 =
0.05136 -0.02038 0.00448 0.00273
AFIX 13
H27 2 -0.906326 -0.846216 -0.625651 21.00000 -1.20000
AFIX 0
C28 1 -0.933420 -0.787813 -0.739090 21.00000 0.04612 0.08859 =
0.04648 -0.01565 0.01209 0.00768
AFIX 23
H28A 2 -0.976513 -0.747689 -0.713453 21.00000 -1.20000
H28B 2 -0.972472 -0.831866 -0.762696 21.00000 -1.20000
AFIX 0
C29 1 -0.876403 -0.748011 -0.810374 21.00000 0.04974 0.08961 =
0.04492 -0.01965 0.00999 0.00365
AFIX 13
H29 2 -0.920159 -0.725404 -0.853991 21.00000 -1.20000
AFIX 0
C30 1 -0.813696 -0.811684 -0.849231 21.00000 0.04151 0.09419 =
0.05310 -0.03693 0.00067 0.00247
AFIX 23
H30A 2 -0.776543 -0.787449 -0.895756 21.00000 -1.20000
H30B 2 -0.853770 -0.854688 -0.873592 21.00000 -1.20000
AFIX 0
C31 1 -0.700449 -0.727993 -0.314349 21.00000 0.04355 0.07265 =
0.02542 -0.00312 0.00550 -0.00785
C32 1 -0.652294 -0.811939 -0.316264 21.00000 0.06813 0.08129 =
0.05060 0.00822 0.01291 0.00099
AFIX 23
H32A 2 -0.636898 -0.826943 -0.375213 21.00000 -1.20000
H32B 2 -0.592711 -0.810522 -0.283388 21.00000 -1.20000
AFIX 0
C33 1 -0.726744 -0.707710 -0.223294 21.00000 0.06438 0.12449 =
0.03764 -0.01081 0.01487 -0.02186
AFIX 23
H33A 2 -0.754897 -0.653204 -0.221053 21.00000 -1.20000
H33B 2 -0.668970 -0.707655 -0.187907 21.00000 -1.20000
AFIX 0
C34 1 -0.790309 -0.730509 -0.370519 21.00000 0.04640 0.05877 =
0.03976 -0.00712 0.00123 -0.00026
AFIX 23
H34A 2 -0.820171 -0.676647 -0.372224 21.00000 -1.20000
H34B 2 -0.773012 -0.745943 -0.428923 21.00000 -1.20000
AFIX 0
C35 1 -0.719847 -0.873500 -0.278223 21.00000 0.07084 0.09209 =
0.06279 0.02793 0.01533 0.00010
AFIX 13
H35 2 -0.690009 -0.928043 -0.279700 21.00000 -1.20000
AFIX 0
C36 1 -0.747462 -0.853075 -0.188835 21.00000 0.05855 0.15023 =
0.06817 0.01574 0.02676 -0.02681
AFIX 23
H36A 2 -0.690372 -0.851193 -0.152628 21.00000 -1.20000
H36B 2 -0.790495 -0.894884 -0.166269 21.00000 -1.20000
AFIX 0
C37 1 -0.798049 -0.769533 -0.187968 21.00000 0.06382 0.13756 =
0.06362 0.00799 0.02480 -0.02099
AFIX 13
H37 2 -0.815776 -0.754830 -0.128784 21.00000 -1.20000
AFIX 0
C38 1 -0.884458 -0.769405 -0.243037 21.00000 0.06956 0.11814 =
0.07611 -0.01104 0.01935 -0.01343
AFIX 23
H38A 2 -0.913544 -0.715217 -0.242259 21.00000 -1.20000
H38B 2 -0.931267 -0.808100 -0.220336 21.00000 -1.20000
AFIX 0
C39 1 -0.860016 -0.792171 -0.333632 21.00000 0.05390 0.06826 =
0.06828 0.00353 0.00692 -0.00454
AFIX 13
H39 2 -0.918791 -0.794221 -0.368762 21.00000 -1.20000
AFIX 0
C40 1 -0.811987 -0.873709 -0.333231 21.00000 0.06692 0.07532 =
0.05957 0.01877 0.01770 -0.00206
AFIX 23
H40A 2 -0.795750 -0.889012 -0.391915 21.00000 -1.20000
H40B 2 -0.856446 -0.914490 -0.310794 21.00000 -1.20000
AFIX 0
N3 4 -0.585707 -0.826593 -0.525135 31.00000 0.06571 0.03463 =
0.05351 0.00473 0.01449 0.01295
C41 1 -0.538434 -0.903691 -0.534653 31.00000 0.05576 0.02708 =
0.09851 -0.00414 0.00566 0.00679
C42 1 -0.514304 -0.922079 -0.628554 31.00000 0.05126 0.04457 =
0.10117 -0.01080 0.01081 0.00900
AFIX 23
H42A 2 -0.573497 -0.924003 -0.661958 31.00000 -1.20000
H42B 2 -0.474383 -0.878288 -0.651532 31.00000 -1.20000
AFIX 0
C43 1 -0.448075 -0.901179 -0.482566 31.00000 0.05447 0.04574 =
0.10499 0.00751 -0.00388 0.00310
AFIX 23
H43A 2 -0.463284 -0.889895 -0.422671 31.00000 -1.20000
H43B 2 -0.405963 -0.857993 -0.503605 31.00000 -1.20000
AFIX 0
C44 1 -0.604378 -0.971690 -0.502590 31.00000 0.04272 0.03151 =
0.11557 -0.00092 0.00529 0.00583
AFIX 23
H44A 2 -0.622085 -0.961258 -0.443074 31.00000 -1.20000
H44B 2 -0.663039 -0.972629 -0.536781 31.00000 -1.20000
AFIX 0
C45 1 -0.462380 -1.001643 -0.637265 31.00000 0.06240 0.04571 =
0.12752 -0.01466 0.00750 0.01524
AFIX 13
H45 2 -0.446482 -1.012569 -0.697751 31.00000 -1.20000
AFIX 0
C46 1 -0.374583 -1.000279 -0.584182 31.00000 0.06300 0.03260 =
0.13022 0.00484 0.00950 -0.00021
AFIX 23
H46A 2 -0.331320 -0.957999 -0.605390 31.00000 -1.20000
H46B 2 -0.341731 -1.052695 -0.588987 31.00000 -1.20000
AFIX 0
C47 1 -0.398180 -0.983645 -0.490245 31.00000 0.04965 0.03901 =
0.13623 0.00585 0.00077 0.00370
AFIX 13
H47 2 -0.338432 -0.983078 -0.456386 31.00000 -1.20000
AFIX 0
C48 1 -0.463567 -1.048579 -0.456864 31.00000 0.05280 0.03789 =
0.16203 0.02031 0.01012 -0.00145
AFIX 23
H48A 2 -0.479830 -1.036774 -0.397301 31.00000 -1.20000
H48B 2 -0.430632 -1.101132 -0.458532 31.00000 -1.20000
AFIX 0
C49 1 -0.554138 -1.053509 -0.509140 31.00000 0.05193 0.03405 =
0.15429 -0.00710 0.01717 0.00516
AFIX 13
H49 2 -0.596017 -1.097233 -0.487091 31.00000 -1.20000
AFIX 0
C50 1 -0.528000 -1.069930 -0.600635 31.00000 0.07056 0.04505 =
0.15939 -0.00726 0.02273 0.01690
AFIX 23
H50A 2 -0.586412 -1.073484 -0.634976 31.00000 -1.20000
H50B 2 -0.494810 -1.122264 -0.604471 31.00000 -1.20000
AFIX 0
PART 0
PART 2
C1A 1 -0.539944 -0.551548 -0.525478 -21.00000 0.03946 0.02410 =
0.05104 -0.00553 -0.00339 0.01259
N1A 4 -0.605011 -0.654242 -0.617230 -21.00000 0.07024 0.02828 =
0.04125 0.00092 -0.00121 0.00549
C2A 1 -0.553208 -0.582421 -0.605691 -21.00000 0.05828 0.02896 =
0.04795 0.00734 -0.00144 0.00915
C3A 1 -0.542818 -0.544682 -0.684544 -21.00000 0.08788 0.04393 =
0.06450 0.02363 -0.01483 -0.00543
AFIX 43
H3A 2 -0.513886 -0.493921 -0.694263 -21.00000 -1.20000
AFIX 0
C4A 1 -0.581016 -0.592926 -0.744232 -21.00000 0.07649 0.05663 =
0.04878 0.02094 -0.00782 -0.00670
AFIX 43
H4A 2 -0.580186 -0.584165 -0.803538 -21.00000 -1.20000
AFIX 0
C5A 1 -0.622216 -0.658543 -0.701899 -21.00000 0.06188 0.04237 =
0.04217 0.00399 -0.00034 0.00224
N2A 4 -0.633752 -0.648321 -0.444031 -21.00000 0.02945 0.03365 =
0.03965 -0.00109 -0.00256 0.00848
C6A 1 -0.577012 -0.578803 -0.449779 -21.00000 0.05362 0.03456 =
0.04857 -0.00804 0.00326 0.00021
C7A 1 -0.588614 -0.532739 -0.373030 -21.00000 0.03657 0.05483 =
0.05364 -0.01870 0.00134 0.01024
AFIX 43
H7A 2 -0.562962 -0.481197 -0.360825 -21.00000 -1.20000
AFIX 0
C8A 1 -0.646423 -0.580740 -0.319717 -21.00000 0.04405 0.07174 =
0.05053 -0.02081 0.00603 -0.00037
AFIX 43
H8A 2 -0.665367 -0.567351 -0.263871 -21.00000 -1.20000
AFIX 0
C9A 1 -0.670953 -0.651398 -0.363378 -21.00000 0.02809 0.05968 =
0.04282 -0.00097 0.00350 0.00769
C11A 1 -0.499661 -0.465980 -0.533708 -21.00000 0.06039 0.03382 =
0.04833 0.00106 0.00390 -0.00238
C12A 1 -0.550223 -0.395793 -0.520578 -21.00000 0.06493 0.03546 =
0.03085 0.00377 0.00246 0.00272
C13A 1 -0.506570 -0.321018 -0.529557 -21.00000 0.07406 0.03062 =
0.07443 0.00079 0.00810 0.00556
C14A 1 -0.411903 -0.314925 -0.546764 -21.00000 0.07262 0.02868 =
0.05819 0.01001 0.01829 -0.00132
C15A 1 -0.357790 -0.382915 -0.548920 -21.00000 0.06136 0.03992 =
0.05640 0.01054 0.02512 -0.00327
C16A 1 -0.404646 -0.456485 -0.543089 -21.00000 0.06440 0.02741 =
0.06837 0.01564 0.00711 0.00352
F1A 3 -0.646103 -0.397925 -0.525334 -21.00000 0.07145 0.04287 =
0.05334 0.01374 0.00545 0.00394
F2A 3 -0.556585 -0.250965 -0.537123 -21.00000 0.08473 0.03372 =
0.04547 0.00254 0.01149 0.00540
F3A 3 -0.363816 -0.243669 -0.541264 -21.00000 0.08496 0.03577 =
0.07364 -0.00258 0.02989 -0.00925
F4A 3 -0.260680 -0.381353 -0.545699 -21.00000 0.06336 0.04721 =
0.08028 0.01200 0.02309 -0.00469
F5A 3 -0.347221 -0.522721 -0.543828 -21.00000 0.06480 0.03493 =
0.07772 0.01207 0.00887 0.00226
C21A 1 -0.684956 -0.722548 -0.741399 -21.00000 0.05934 0.05875 =
0.04309 -0.01297 0.00164 -0.00070
C22A 1 -0.638491 -0.806164 -0.737593 -21.00000 0.04420 0.05983 =
0.04084 -0.01610 0.00177 -0.00194
AFIX 23
H22C 2 -0.579905 -0.805665 -0.771896 -21.00000 -1.20000
H22D 2 -0.620594 -0.818149 -0.678445 -21.00000 -1.20000
AFIX 0
C23A 1 -0.778459 -0.725073 -0.693905 -21.00000 0.06397 0.05294 =
0.05041 -0.01506 0.01058 0.00207
AFIX 23
H23C 2 -0.809633 -0.671885 -0.698226 -21.00000 -1.20000
H23D 2 -0.765924 -0.735765 -0.633400 -21.00000 -1.20000
AFIX 0
C24A 1 -0.708842 -0.701215 -0.834828 -21.00000 0.05639 0.08057 =
0.04647 -0.00760 0.00188 -0.00213
AFIX 23
H24C 2 -0.741396 -0.648529 -0.837519 -21.00000 -1.20000
H24D 2 -0.649962 -0.697736 -0.868533 -21.00000 -1.20000
AFIX 0
C25A 1 -0.703846 -0.872320 -0.770012 -21.00000 0.04530 0.06941 =
0.07262 -0.02945 -0.00058 -0.00462
AFIX 13
H25A 2 -0.672072 -0.926014 -0.767105 -21.00000 -1.20000
AFIX 0
C26A 1 -0.794480 -0.872633 -0.720623 -21.00000 0.04371 0.06405 =
0.07147 -0.03184 0.00354 -0.00902
AFIX 23
H26C 2 -0.780801 -0.884214 -0.660497 -21.00000 -1.20000
H26D 2 -0.836604 -0.915515 -0.742318 -21.00000 -1.20000
AFIX 0
C27A 1 -0.845146 -0.789554 -0.728128 -21.00000 0.05327 0.06254 =
0.05136 -0.02038 0.00448 0.00273
AFIX 13
H27A 2 -0.905386 -0.789990 -0.694968 -21.00000 -1.20000
AFIX 0
C28A 1 -0.865756 -0.773070 -0.820591 -21.00000 0.04612 0.08859 =
0.04648 -0.01565 0.01209 0.00768
AFIX 23
H28C 2 -0.901564 -0.722134 -0.826051 -21.00000 -1.20000
H28D 2 -0.905023 -0.817036 -0.844089 -21.00000 -1.20000
AFIX 0
C29A 1 -0.772831 -0.766979 -0.870118 -21.00000 0.04974 0.08961 =
0.04492 -0.01965 0.00999 0.00365
AFIX 13
H29A 2 -0.787436 -0.754660 -0.930568 -21.00000 -1.20000
AFIX 0
C30A 1 -0.727030 -0.848836 -0.864833 -21.00000 0.04151 0.09419 =
0.05310 -0.03693 0.00067 0.00247
AFIX 23
H30C 2 -0.667809 -0.848757 -0.898259 -21.00000 -1.20000
H30D 2 -0.770032 -0.889584 -0.889489 -21.00000 -1.20000
AFIX 0
C31A 1 -0.732085 -0.721472 -0.337558 -21.00000 0.04355 0.07265 =
0.02542 -0.00312 0.00550 -0.00785
C32A 1 -0.670164 -0.793192 -0.308313 -21.00000 0.06813 0.08129 =
0.05060 0.00822 0.01291 0.00099
AFIX 23
H32C 2 -0.628514 -0.810514 -0.355206 -21.00000 -1.20000
H32D 2 -0.629579 -0.776174 -0.260562 -21.00000 -1.20000
AFIX 0
C33A 1 -0.797354 -0.696799 -0.266145 -21.00000 0.06438 0.12449 =
0.03764 -0.01081 0.01487 -0.02186
AFIX 23
H33C 2 -0.837462 -0.651263 -0.284695 -21.00000 -1.20000
H33D 2 -0.759204 -0.678636 -0.217272 -21.00000 -1.20000
AFIX 0
C34A 1 -0.794805 -0.750582 -0.412461 -21.00000 0.04640 0.05877 =
0.03976 -0.00712 0.00123 -0.00026
AFIX 23
H34C 2 -0.835719 -0.705815 -0.431660 -21.00000 -1.20000
H34D 2 -0.753775 -0.766610 -0.460288 -21.00000 -1.20000
AFIX 0
C35A 1 -0.732408 -0.863151 -0.280885 -21.00000 0.07084 0.09209 =
0.06279 0.02793 0.01533 0.00010
AFIX 13
H35A 2 -0.691423 -0.908621 -0.261560 -21.00000 -1.20000
AFIX 0
C36A 1 -0.795932 -0.837629 -0.209710 -21.00000 0.05855 0.15023 =
0.06817 0.01574 0.02676 -0.02681
AFIX 23
H36C 2 -0.757217 -0.820089 -0.160940 -21.00000 -1.20000
H36D 2 -0.835517 -0.883622 -0.191510 -21.00000 -1.20000
AFIX 0
C37A 1 -0.860357 -0.767276 -0.239419 -21.00000 0.06382 0.13756 =
0.06362 0.00799 0.02480 -0.02099
AFIX 13
H37A 2 -0.903098 -0.750266 -0.192336 -21.00000 -1.20000
AFIX 0
C38A 1 -0.918592 -0.794666 -0.314375 -21.00000 0.06956 0.11814 =
0.07611 -0.01104 0.01935 -0.01343
AFIX 23
H38C 2 -0.960246 -0.839584 -0.296909 -21.00000 -1.20000
H38D 2 -0.959307 -0.749802 -0.333661 -21.00000 -1.20000
AFIX 0
C39A 1 -0.856509 -0.821853 -0.386337 -21.00000 0.05390 0.06826 =
0.06828 0.00353 0.00692 -0.00454
AFIX 13
H39A 2 -0.896666 -0.839243 -0.435051 -21.00000 -1.20000
AFIX 0
C40A 1 -0.792608 -0.891156 -0.358570 -21.00000 0.06692 0.07532 =
0.05957 0.01877 0.01770 -0.00206
AFIX 23
H40C 2 -0.750277 -0.906951 -0.405572 -21.00000 -1.20000
H40D 2 -0.831577 -0.938354 -0.342888 -21.00000 -1.20000
AFIX 0
N3A 4 -0.585707 -0.826593 -0.525135 -31.00000 0.06571 0.03463 =
0.05351 0.00473 0.01449 0.01295
C41A 1 -0.535304 -0.902529 -0.532997 -31.00000 0.05576 0.02708 =
0.09851 -0.00414 0.00566 0.00679
C42A 1 -0.448465 -0.894530 -0.592917 -31.00000 0.05126 0.04457 =
0.10117 -0.01080 0.01081 0.00900
AFIX 23
H42C 2 -0.470532 -0.879728 -0.650210 -31.00000 -1.20000
H42D 2 -0.406692 -0.850945 -0.572249 -31.00000 -1.20000
AFIX 0
C43A 1 -0.502195 -0.924653 -0.445284 -31.00000 0.05447 0.04574 =
0.10499 0.00751 -0.00388 0.00310
AFIX 23
H43C 2 -0.557389 -0.930090 -0.407180 -31.00000 -1.20000
H43D 2 -0.460739 -0.881675 -0.422788 -31.00000 -1.20000
AFIX 0
C44A 1 -0.600895 -0.969941 -0.568278 -31.00000 0.04272 0.03151 =
0.11557 -0.00092 0.00529 0.00583
AFIX 23
H44C 2 -0.656803 -0.976355 -0.531183 -31.00000 -1.20000
H44D 2 -0.623317 -0.955149 -0.625464 -31.00000 -1.20000
AFIX 0
C45A 1 -0.392594 -0.972657 -0.597573 -31.00000 0.06240 0.04571 =
0.12752 -0.01466 0.00750 0.01524
AFIX 13
H45A 2 -0.336356 -0.966447 -0.635372 -31.00000 -1.20000
AFIX 0
C46A 1 -0.362761 -0.996106 -0.511071 -31.00000 0.06300 0.03260 =
0.13022 0.00484 0.00950 -0.00021
AFIX 23
H46C 2 -0.318289 -0.955163 -0.488984 -31.00000 -1.20000
H46D 2 -0.328566 -1.048027 -0.513914 -31.00000 -1.20000
AFIX 0
C47A 1 -0.447516 -1.004529 -0.448639 -31.00000 0.04965 0.03901 =
0.13623 0.00585 0.00077 0.00370
AFIX 13
H47A 2 -0.424255 -1.019419 -0.391056 -31.00000 -1.20000
AFIX 0
C48A 1 -0.511796 -1.069302 -0.482748 -31.00000 0.05280 0.03789 =
0.16203 0.02031 0.01012 -0.00145
AFIX 23
H48C 2 -0.567545 -1.074835 -0.445309 -31.00000 -1.20000
H48D 2 -0.477658 -1.121321 -0.482968 -31.00000 -1.20000
AFIX 0
C49A 1 -0.544931 -1.049841 -0.572252 -31.00000 0.05193 0.03405 =
0.15429 -0.00710 0.01717 0.00516
AFIX 13
H49A 2 -0.587125 -1.093820 -0.593239 -31.00000 -1.20000
AFIX 0
C50A 1 -0.461693 -1.039105 -0.632757 -31.00000 0.07056 0.04505 =
0.15939 -0.00726 0.02273 0.01690
AFIX 23
H50C 2 -0.485311 -1.022956 -0.689149 -31.00000 -1.20000
H50D 2 -0.427332 -1.090693 -0.638841 -31.00000 -1.20000
AFIX 0
HKLF 4
REM 4.res in Pna2(1)
REM R1 = 0.0792 for 3085 Fo > 4sig(Fo) and 0.1623 for all 6222 data
REM 631 parameters refined using 1015 restraints
END
WGHT 0.0908 6.2670
REM Highest difference peak 0.532, deepest hole -0.762, 1-sigma level 0.084
Q1 1 -0.7332 -0.7324 -0.5243 11.00000 0.05 0.53
;
_shelx_res_checksum 73740
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_LNiPy
_database_code_depnum_ccdc_archive 'CCDC 1953730'
loop_
_audit_author_name
_audit_author_address
'Shao-Liang Zheng'
;Harvard Univerisity
United States of America
;
_audit_update_record
;
2019-09-16 deposited with the CCDC. 2019-12-09 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C40 H39 F5 N3 Ni'
_chemical_formula_weight 715.45
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 17.7017(3)
_cell_length_b 15.1269(2)
_cell_length_c 13.1410(2)
_cell_angle_alpha 90
_cell_angle_beta 109.571(2)
_cell_angle_gamma 90
_cell_volume 3315.50(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9959
_cell_measurement_theta_min 2.65
_cell_measurement_theta_max 66.64
_exptl_crystal_description plate
_exptl_crystal_colour brown
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.433
_exptl_crystal_F_000 1492
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.420
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.080
_exptl_absorpt_coefficient_mu 1.374
_shelx_estimated_absorpt_T_min 0.596
_shelx_estimated_absorpt_T_max 0.898
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5853
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details SADBAS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source 'I/mS microfocus tube'
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 42106
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_av_R_equivalents 0.0752
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.649
_diffrn_reflns_theta_max 66.787
_diffrn_reflns_theta_full 66.787
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total 5677
_reflns_number_gt 4658
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_cell_refinement 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_reduction 'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. All non H-atoms were located in difference-Fourier maps, and then refined anisotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+1.3876P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 5677
_refine_ls_number_parameters 442
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0558
_refine_ls_R_factor_gt 0.0444
_refine_ls_wR_factor_ref 0.1266
_refine_ls_wR_factor_gt 0.1174
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_restrained_S_all 1.036
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.71715(2) 0.25993(2) 0.76149(3) 0.02434(13) Uani 1 1 d . . . . .
F1 F 0.73557(10) 0.62837(9) 0.71777(11) 0.0394(4) Uani 1 1 d . . . . .
F5 F 0.75383(9) 0.48337(9) 1.04317(11) 0.0370(3) Uani 1 1 d . . . . .
F4 F 0.77958(10) 0.63908(10) 1.14653(12) 0.0442(4) Uani 1 1 d . . . . .
F2 F 0.75272(10) 0.78518(9) 0.82080(13) 0.0456(4) Uani 1 1 d . . . . .
F3 F 0.77295(10) 0.79183(10) 1.03343(13) 0.0451(4) Uani 1 1 d . . . . .
N2 N 0.64781(11) 0.35789(11) 0.69756(14) 0.0229(4) Uani 1 1 d . . . . .
N1 N 0.81790(11) 0.32970(12) 0.81579(15) 0.0267(4) Uani 1 1 d . . . . .
N3 N 0.73150(11) 0.15196(12) 0.84789(16) 0.0273(4) Uani 1 1 d . . . . .
C9 C 0.57142(13) 0.36051(14) 0.62966(17) 0.0234(5) Uani 1 1 d . . . . .
C11 C 0.74464(13) 0.55085(15) 0.87753(18) 0.0270(5) Uani 1 1 d . . . . .
C31 C 0.53541(13) 0.28525(14) 0.55381(17) 0.0232(5) Uani 1 1 d . . . . .
C16 C 0.75562(14) 0.55704(16) 0.98654(19) 0.0299(5) Uani 1 1 d . . . . .
C6 C 0.66224(13) 0.43878(14) 0.75206(18) 0.0250(5) Uani 1 1 d . . . . .
C8 C 0.53516(14) 0.44273(15) 0.63933(18) 0.0277(5) Uani 1 1 d . . . . .
H8 H 0.4819 0.4606 0.5999 0.033 Uiso 1 1 calc R U . . .
C15 C 0.76790(14) 0.63637(17) 1.04107(19) 0.0322(5) Uani 1 1 d . . . . .
C12 C 0.74415(15) 0.62939(15) 0.82291(19) 0.0295(5) Uani 1 1 d . . . . .
C13 C 0.75417(15) 0.71022(16) 0.8753(2) 0.0329(5) Uani 1 1 d . . . . .
C1 C 0.73781(14) 0.46198(14) 0.82420(18) 0.0263(5) Uani 1 1 d . . . . .
C5 C 0.89729(14) 0.31519(16) 0.84284(19) 0.0307(5) Uani 1 1 d . . . . .
C33 C 0.55359(14) 0.19610(14) 0.61436(18) 0.0262(5) Uani 1 1 d . . . . .
H33A H 0.6123 0.1886 0.6477 0.031 Uiso 1 1 calc R U . . .
H33B H 0.5299 0.1958 0.6728 0.031 Uiso 1 1 calc R U . . .
C32 C 0.44398(13) 0.29511(15) 0.50314(18) 0.0264(5) Uani 1 1 d . . . . .
H32A H 0.4196 0.2957 0.5608 0.032 Uiso 1 1 calc R U . . .
H32B H 0.4311 0.3518 0.4635 0.032 Uiso 1 1 calc R U . . .
C45 C 0.75885(14) 0.16200(16) 0.95584(19) 0.0298(5) Uani 1 1 d . . . . .
H45 H 0.7772 0.2189 0.9841 0.036 Uiso 1 1 calc R U . . .
C2 C 0.80961(14) 0.41536(15) 0.85028(18) 0.0280(5) Uani 1 1 d . . . . .
C34 C 0.57204(14) 0.28270(16) 0.46294(19) 0.0290(5) Uani 1 1 d . . . . .
H34A H 0.5609 0.3392 0.4227 0.035 Uiso 1 1 calc R U . . .
H34B H 0.6309 0.2757 0.4947 0.035 Uiso 1 1 calc R U . . .
C38 C 0.42786(14) 0.13067(15) 0.4880(2) 0.0298(5) Uani 1 1 d . . . . .
H38A H 0.4041 0.1311 0.5463 0.036 Uiso 1 1 calc R U . . .
H38B H 0.4043 0.0807 0.4389 0.036 Uiso 1 1 calc R U . . .
C35 C 0.53718(15) 0.20607(16) 0.3850(2) 0.0322(5) Uani 1 1 d . . . . .
H35 H 0.5614 0.2059 0.3263 0.039 Uiso 1 1 calc R U . . .
C39 C 0.51896(14) 0.11909(15) 0.53663(19) 0.0288(5) Uani 1 1 d . . . . .
H39 H 0.5314 0.0620 0.5772 0.035 Uiso 1 1 calc R U . . .
C7 C 0.59164(14) 0.49113(15) 0.71624(18) 0.0283(5) Uani 1 1 d . . . . .
H7 H 0.5848 0.5487 0.7408 0.034 Uiso 1 1 calc R U . . .
C14 C 0.76538(15) 0.71334(17) 0.9836(2) 0.0345(6) Uani 1 1 d . . . . .
C37 C 0.40912(14) 0.21814(15) 0.42520(19) 0.0292(5) Uani 1 1 d . . . . .
H37 H 0.3497 0.2254 0.3926 0.035 Uiso 1 1 calc R U . . .
C4 C 0.94101(15) 0.39047(18) 0.8960(2) 0.0363(6) Uani 1 1 d . . . . .
H4 H 0.9977 0.3966 0.9223 0.044 Uiso 1 1 calc R U . . .
C40 C 0.55605(15) 0.11874(16) 0.4473(2) 0.0334(5) Uani 1 1 d . . . . .
H40A H 0.5342 0.0688 0.3974 0.040 Uiso 1 1 calc R U . . .
H40B H 0.6148 0.1110 0.4791 0.040 Uiso 1 1 calc R U . . .
C44 C 0.76182(15) 0.09475(18) 1.0281(2) 0.0375(6) Uani 1 1 d . . . . .
H44 H 0.7823 0.1051 1.1037 0.045 Uiso 1 1 calc R U . . .
C3 C 0.88695(14) 0.45197(17) 0.9024(2) 0.0339(5) Uani 1 1 d . . . . .
H3 H 0.8985 0.5086 0.9353 0.041 Uiso 1 1 calc R U . . .
C36 C 0.44621(16) 0.21719(16) 0.33560(19) 0.0337(6) Uani 1 1 d . . . . .
H36A H 0.4336 0.2732 0.2944 0.040 Uiso 1 1 calc R U . . .
H36B H 0.4233 0.1679 0.2852 0.040 Uiso 1 1 calc R U . . .
C21 C 0.93359(15) 0.23261(17) 0.8140(2) 0.0332(6) Uani 1 1 d . . . . .
C22 C 0.88394(16) 0.20354(18) 0.6984(2) 0.0373(6) Uani 1 1 d . . . . .
H22A H 0.8283 0.1905 0.6947 0.045 Uiso 1 1 calc R U . . .
H22B H 0.8822 0.2522 0.6472 0.045 Uiso 1 1 calc R U . . .
C23 C 0.93676(16) 0.15543(18) 0.8924(2) 0.0392(6) Uani 1 1 d . . . . .
H23A H 0.9698 0.1727 0.9666 0.047 Uiso 1 1 calc R U . . .
H23B H 0.8820 0.1421 0.8921 0.047 Uiso 1 1 calc R U . . .
C41 C 0.70637(18) 0.07094(17) 0.8104(2) 0.0445(7) Uani 1 1 d . . . . .
H41 H 0.6874 0.0618 0.7345 0.053 Uiso 1 1 calc R U . . .
C24 C 1.02025(16) 0.25150(19) 0.8176(2) 0.0414(6) Uani 1 1 d . . . . .
H24A H 1.0200 0.3008 0.7680 0.050 Uiso 1 1 calc R U . . .
H24B H 1.0533 0.2695 0.8916 0.050 Uiso 1 1 calc R U . . .
C29 C 0.97279(18) 0.0729(2) 0.8586(3) 0.0500(7) Uani 1 1 d . . . . .
H29 H 0.9739 0.0234 0.9095 0.060 Uiso 1 1 calc R U . . .
C26 C 1.00623(18) 0.1425(2) 0.6706(3) 0.0509(8) Uani 1 1 d . . . . .
H26A H 1.0300 0.0900 0.6480 0.061 Uiso 1 1 calc R U . . .
H26B H 1.0053 0.1914 0.6201 0.061 Uiso 1 1 calc R U . . .
C27 C 0.92072(17) 0.1215(2) 0.6660(2) 0.0456(7) Uani 1 1 d . . . . .
H27 H 0.8880 0.1036 0.5908 0.055 Uiso 1 1 calc R U . . .
C25 C 1.05701(17) 0.1689(2) 0.7845(3) 0.0510(8) Uani 1 1 d . . . . .
H25 H 1.1128 0.1825 0.7866 0.061 Uiso 1 1 calc R U . . .
C43 C 0.73460(18) 0.01273(19) 0.9884(3) 0.0497(7) Uani 1 1 d . . . . .
H43 H 0.7348 -0.0346 1.0359 0.060 Uiso 1 1 calc R U . . .
C42 C 0.7067(2) -0.00006(18) 0.8771(3) 0.0572(9) Uani 1 1 d . . . . .
H42 H 0.6882 -0.0565 0.8474 0.069 Uiso 1 1 calc R U . . .
C28 C 0.92146(18) 0.0465(2) 0.7442(3) 0.0495(7) Uani 1 1 d . . . . .
H28A H 0.8660 0.0338 0.7419 0.059 Uiso 1 1 calc R U . . .
H28B H 0.9435 -0.0078 0.7226 0.059 Uiso 1 1 calc R U . . .
C30 C 1.05898(18) 0.0933(2) 0.8619(3) 0.0561(8) Uani 1 1 d . . . . .
H30A H 1.0925 0.1100 0.9361 0.067 Uiso 1 1 calc R U . . .
H30B H 1.0827 0.0401 0.8406 0.067 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0217(2) 0.0235(2) 0.0246(2) -0.00003(14) 0.00359(16) 0.00031(15)
F1 0.0567(10) 0.0321(8) 0.0284(8) 0.0012(5) 0.0130(7) -0.0077(7)
F5 0.0443(9) 0.0375(8) 0.0290(7) 0.0053(6) 0.0121(6) 0.0035(6)
F4 0.0480(10) 0.0535(9) 0.0275(8) -0.0061(6) 0.0079(7) 0.0103(7)
F2 0.0586(11) 0.0279(8) 0.0465(9) 0.0011(6) 0.0126(8) -0.0087(7)
F3 0.0466(10) 0.0363(8) 0.0463(9) -0.0160(7) 0.0075(7) -0.0037(7)
N2 0.0232(10) 0.0226(9) 0.0204(9) 0.0003(7) 0.0039(7) -0.0029(7)
N1 0.0220(10) 0.0308(10) 0.0253(10) 0.0009(7) 0.0053(8) -0.0014(8)
N3 0.0237(10) 0.0250(10) 0.0292(11) -0.0008(7) 0.0036(8) 0.0036(8)
C9 0.0228(11) 0.0254(11) 0.0203(11) 0.0037(8) 0.0049(9) -0.0008(9)
C11 0.0250(12) 0.0266(11) 0.0268(12) -0.0021(9) 0.0054(9) -0.0034(9)
C31 0.0222(12) 0.0230(11) 0.0222(11) 0.0018(8) 0.0045(9) 0.0001(9)
C16 0.0249(12) 0.0339(13) 0.0290(13) 0.0017(9) 0.0066(9) 0.0017(10)
C6 0.0289(12) 0.0225(11) 0.0229(11) 0.0008(8) 0.0077(9) -0.0033(9)
C8 0.0267(12) 0.0255(11) 0.0264(12) 0.0022(9) 0.0030(9) 0.0043(9)
C15 0.0271(13) 0.0423(14) 0.0232(13) -0.0051(9) 0.0031(9) 0.0029(10)
C12 0.0319(13) 0.0308(12) 0.0239(13) -0.0017(9) 0.0068(9) -0.0055(10)
C13 0.0307(13) 0.0273(12) 0.0368(15) 0.0021(10) 0.0063(10) -0.0040(10)
C1 0.0316(13) 0.0248(11) 0.0225(12) 0.0003(8) 0.0090(9) -0.0043(9)
C5 0.0226(12) 0.0405(13) 0.0290(13) 0.0003(10) 0.0087(9) -0.0017(10)
C33 0.0264(12) 0.0250(11) 0.0241(12) 0.0012(9) 0.0045(9) 0.0019(9)
C32 0.0220(12) 0.0264(11) 0.0277(12) 0.0020(9) 0.0042(9) 0.0016(9)
C45 0.0296(13) 0.0300(12) 0.0289(13) 0.0018(9) 0.0086(10) 0.0067(10)
C2 0.0300(12) 0.0308(12) 0.0222(12) -0.0004(8) 0.0073(9) -0.0053(10)
C34 0.0258(12) 0.0321(12) 0.0291(13) 0.0002(9) 0.0089(10) -0.0024(10)
C38 0.0284(13) 0.0267(12) 0.0322(13) -0.0030(9) 0.0072(10) -0.0049(9)
C35 0.0354(14) 0.0364(13) 0.0276(13) -0.0064(10) 0.0145(10) -0.0044(11)
C39 0.0295(13) 0.0213(11) 0.0318(13) 0.0004(9) 0.0054(10) 0.0001(9)
C7 0.0336(13) 0.0217(11) 0.0273(12) 0.0001(8) 0.0073(10) 0.0013(9)
C14 0.0275(13) 0.0336(13) 0.0389(15) -0.0119(10) 0.0063(10) -0.0035(10)
C37 0.0229(12) 0.0306(12) 0.0288(13) -0.0012(9) 0.0017(9) -0.0012(9)
C4 0.0247(13) 0.0467(15) 0.0360(14) -0.0050(11) 0.0084(10) -0.0085(11)
C40 0.0307(13) 0.0299(12) 0.0379(14) -0.0088(10) 0.0094(11) 0.0002(10)
C44 0.0327(14) 0.0444(15) 0.0353(14) 0.0094(11) 0.0114(11) 0.0136(11)
C3 0.0295(13) 0.0356(13) 0.0351(14) -0.0054(10) 0.0088(10) -0.0114(10)
C36 0.0383(15) 0.0333(13) 0.0238(13) -0.0044(9) 0.0030(10) -0.0060(11)
C21 0.0230(13) 0.0445(14) 0.0300(14) -0.0025(10) 0.0059(10) 0.0031(10)
C22 0.0295(14) 0.0469(15) 0.0332(14) -0.0051(11) 0.0077(10) 0.0025(11)
C23 0.0303(14) 0.0482(15) 0.0349(14) 0.0013(11) 0.0053(11) 0.0048(12)
C41 0.0476(17) 0.0286(13) 0.0426(16) -0.0010(10) -0.0044(12) 0.0046(12)
C24 0.0239(14) 0.0591(18) 0.0385(15) -0.0050(12) 0.0070(11) 0.0008(12)
C29 0.0446(17) 0.0458(17) 0.0550(19) 0.0056(13) 0.0105(14) 0.0146(14)
C26 0.0377(16) 0.0637(19) 0.0531(19) -0.0127(14) 0.0175(13) 0.0104(14)
C27 0.0370(16) 0.0570(18) 0.0402(16) -0.0134(12) 0.0095(12) 0.0060(13)
C25 0.0265(15) 0.070(2) 0.0550(19) -0.0080(15) 0.0121(13) 0.0078(14)
C43 0.0460(17) 0.0385(15) 0.0588(19) 0.0226(13) 0.0101(14) 0.0074(13)
C42 0.058(2) 0.0236(14) 0.069(2) 0.0083(12) -0.0063(15) -0.0022(13)
C28 0.0393(16) 0.0446(16) 0.0612(19) -0.0119(13) 0.0124(14) 0.0104(13)
C30 0.0356(16) 0.063(2) 0.060(2) -0.0057(15) 0.0033(14) 0.0194(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.9281(18) . ?
Ni1 N3 1.9566(19) . ?
Ni1 N1 1.9878(19) . ?
F1 C12 1.339(3) . ?
F5 C16 1.346(3) . ?
F4 C15 1.332(3) . ?
F2 C13 1.337(3) . ?
F3 C14 1.341(3) . ?
N2 C9 1.348(3) . ?
N2 C6 1.397(3) . ?
N1 C5 1.347(3) . ?
N1 C2 1.397(3) . ?
N3 C41 1.340(3) . ?
N3 C45 1.345(3) . ?
C9 C8 1.425(3) . ?
C9 C31 1.507(3) . ?
C11 C16 1.383(3) . ?
C11 C12 1.387(3) . ?
C11 C1 1.502(3) . ?
C31 C32 1.537(3) . ?
C31 C34 1.538(3) . ?
C31 C33 1.544(3) . ?
C16 C15 1.377(3) . ?
C6 C1 1.401(3) . ?
C6 C7 1.420(3) . ?
C8 C7 1.371(3) . ?
C8 H8 0.9500 . ?
C15 C14 1.380(4) . ?
C12 C13 1.385(3) . ?
C13 C14 1.371(4) . ?
C1 C2 1.392(3) . ?
C5 C4 1.422(3) . ?
C5 C21 1.510(3) . ?
C33 C39 1.535(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C32 C37 1.537(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C45 C44 1.381(4) . ?
C45 H45 0.9500 . ?
C2 C3 1.422(3) . ?
C34 C35 1.533(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C38 C39 1.533(3) . ?
C38 C37 1.536(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C35 C36 1.530(3) . ?
C35 C40 1.531(3) . ?
C35 H35 1.0000 . ?
C39 C40 1.526(4) . ?
C39 H39 1.0000 . ?
C7 H7 0.9500 . ?
C37 C36 1.528(4) . ?
C37 H37 1.0000 . ?
C4 C3 1.357(4) . ?
C4 H4 0.9500 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C44 C43 1.370(4) . ?
C44 H44 0.9500 . ?
C3 H3 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C21 C22 1.543(3) . ?
C21 C24 1.545(3) . ?
C21 C23 1.546(4) . ?
C22 C27 1.527(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C29 1.533(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C41 C42 1.385(4) . ?
C41 H41 0.9500 . ?
C24 C25 1.537(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C29 C28 1.527(4) . ?
C29 C30 1.543(4) . ?
C29 H29 1.0000 . ?
C26 C25 1.519(4) . ?
C26 C27 1.528(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.528(4) . ?
C27 H27 1.0000 . ?
C25 C30 1.523(5) . ?
C25 H25 1.0000 . ?
C43 C42 1.391(5) . ?
C43 H43 0.9500 . ?
C42 H42 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N3 146.55(8) . . ?
N2 Ni1 N1 96.43(8) . . ?
N3 Ni1 N1 107.97(8) . . ?
C9 N2 C6 106.50(18) . . ?
C9 N2 Ni1 131.45(15) . . ?
C6 N2 Ni1 117.98(14) . . ?
C5 N1 C2 106.22(19) . . ?
C5 N1 Ni1 137.68(17) . . ?
C2 N1 Ni1 115.46(15) . . ?
C41 N3 C45 116.7(2) . . ?
C41 N3 Ni1 126.00(17) . . ?
C45 N3 Ni1 116.65(15) . . ?
N2 C9 C8 110.40(19) . . ?
N2 C9 C31 121.59(19) . . ?
C8 C9 C31 127.97(19) . . ?
C16 C11 C12 116.9(2) . . ?
C16 C11 C1 120.4(2) . . ?
C12 C11 C1 122.7(2) . . ?
C9 C31 C32 111.34(18) . . ?
C9 C31 C34 109.73(18) . . ?
C32 C31 C34 108.82(18) . . ?
C9 C31 C33 110.49(18) . . ?
C32 C31 C33 108.39(18) . . ?
C34 C31 C33 107.98(18) . . ?
F5 C16 C15 117.6(2) . . ?
F5 C16 C11 119.7(2) . . ?
C15 C16 C11 122.8(2) . . ?
N2 C6 C1 122.4(2) . . ?
N2 C6 C7 109.20(19) . . ?
C1 C6 C7 128.3(2) . . ?
C7 C8 C9 107.0(2) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
F4 C15 C16 120.7(2) . . ?
F4 C15 C14 120.6(2) . . ?
C16 C15 C14 118.7(2) . . ?
F1 C12 C13 118.3(2) . . ?
F1 C12 C11 120.2(2) . . ?
C13 C12 C11 121.5(2) . . ?
F2 C13 C14 119.8(2) . . ?
F2 C13 C12 120.4(2) . . ?
C14 C13 C12 119.7(2) . . ?
C2 C1 C6 128.7(2) . . ?
C2 C1 C11 114.5(2) . . ?
C6 C1 C11 116.7(2) . . ?
N1 C5 C4 110.3(2) . . ?
N1 C5 C21 124.2(2) . . ?
C4 C5 C21 125.4(2) . . ?
C39 C33 C31 110.62(18) . . ?
C39 C33 H33A 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C39 C33 H33B 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C37 C32 C31 110.16(18) . . ?
C37 C32 H32A 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C37 C32 H32B 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
N3 C45 C44 124.0(2) . . ?
N3 C45 H45 118.0 . . ?
C44 C45 H45 118.0 . . ?
C1 C2 N1 125.2(2) . . ?
C1 C2 C3 125.0(2) . . ?
N1 C2 C3 109.2(2) . . ?
C35 C34 C31 110.97(19) . . ?
C35 C34 H34A 109.4 . . ?
C31 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C31 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C39 C38 C37 109.27(19) . . ?
C39 C38 H38A 109.8 . . ?
C37 C38 H38A 109.8 . . ?
C39 C38 H38B 109.8 . . ?
C37 C38 H38B 109.8 . . ?
H38A C38 H38B 108.3 . . ?
C36 C35 C40 109.4(2) . . ?
C36 C35 C34 109.3(2) . . ?
C40 C35 C34 109.2(2) . . ?
C36 C35 H35 109.7 . . ?
C40 C35 H35 109.7 . . ?
C34 C35 H35 109.7 . . ?
C40 C39 C38 110.10(19) . . ?
C40 C39 C33 109.63(19) . . ?
C38 C39 C33 108.70(19) . . ?
C40 C39 H39 109.5 . . ?
C38 C39 H39 109.5 . . ?
C33 C39 H39 109.5 . . ?
C8 C7 C6 106.9(2) . . ?
C8 C7 H7 126.6 . . ?
C6 C7 H7 126.6 . . ?
F3 C14 C13 119.6(2) . . ?
F3 C14 C15 120.0(2) . . ?
C13 C14 C15 120.4(2) . . ?
C36 C37 C38 109.6(2) . . ?
C36 C37 C32 109.90(19) . . ?
C38 C37 C32 109.16(19) . . ?
C36 C37 H37 109.4 . . ?
C38 C37 H37 109.4 . . ?
C32 C37 H37 109.4 . . ?
C3 C4 C5 107.5(2) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
C39 C40 C35 109.61(19) . . ?
C39 C40 H40A 109.7 . . ?
C35 C40 H40A 109.7 . . ?
C39 C40 H40B 109.7 . . ?
C35 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
C43 C44 C45 118.5(3) . . ?
C43 C44 H44 120.7 . . ?
C45 C44 H44 120.7 . . ?
C4 C3 C2 106.8(2) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
C37 C36 C35 109.70(19) . . ?
C37 C36 H36A 109.7 . . ?
C35 C36 H36A 109.7 . . ?
C37 C36 H36B 109.7 . . ?
C35 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C5 C21 C22 109.5(2) . . ?
C5 C21 C24 109.9(2) . . ?
C22 C21 C24 108.4(2) . . ?
C5 C21 C23 112.4(2) . . ?
C22 C21 C23 108.8(2) . . ?
C24 C21 C23 107.8(2) . . ?
C27 C22 C21 110.5(2) . . ?
C27 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C27 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C29 C23 C21 110.4(2) . . ?
C29 C23 H23A 109.6 . . ?
C21 C23 H23A 109.6 . . ?
C29 C23 H23B 109.6 . . ?
C21 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
N3 C41 C42 123.1(3) . . ?
N3 C41 H41 118.4 . . ?
C42 C41 H41 118.4 . . ?
C25 C24 C21 110.5(2) . . ?
C25 C24 H24A 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C28 C29 C23 109.3(2) . . ?
C28 C29 C30 109.6(3) . . ?
C23 C29 C30 109.4(3) . . ?
C28 C29 H29 109.5 . . ?
C23 C29 H29 109.5 . . ?
C30 C29 H29 109.5 . . ?
C25 C26 C27 110.2(3) . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C22 C27 C26 109.2(2) . . ?
C22 C27 C28 108.9(2) . . ?
C26 C27 C28 110.1(3) . . ?
C22 C27 H27 109.6 . . ?
C26 C27 H27 109.6 . . ?
C28 C27 H27 109.6 . . ?
C26 C25 C30 109.5(3) . . ?
C26 C25 C24 109.0(2) . . ?
C30 C25 C24 109.8(3) . . ?
C26 C25 H25 109.5 . . ?
C30 C25 H25 109.5 . . ?
C24 C25 H25 109.5 . . ?
C44 C43 C42 118.8(3) . . ?
C44 C43 H43 120.6 . . ?
C42 C43 H43 120.6 . . ?
C41 C42 C43 118.8(3) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C29 C28 C27 109.6(2) . . ?
C29 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
C29 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C25 C30 C29 109.3(2) . . ?
C25 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
C25 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.3 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 C9 C8 -0.2(2) . . . . ?
Ni1 N2 C9 C8 155.92(17) . . . . ?
C6 N2 C9 C31 177.62(19) . . . . ?
Ni1 N2 C9 C31 -26.2(3) . . . . ?
N2 C9 C31 C32 167.93(19) . . . . ?
C8 C9 C31 C32 -14.7(3) . . . . ?
N2 C9 C31 C34 -71.5(3) . . . . ?
C8 C9 C31 C34 105.9(3) . . . . ?
N2 C9 C31 C33 47.4(3) . . . . ?
C8 C9 C31 C33 -135.2(2) . . . . ?
C12 C11 C16 F5 177.7(2) . . . . ?
C1 C11 C16 F5 -5.2(3) . . . . ?
C12 C11 C16 C15 -1.8(4) . . . . ?
C1 C11 C16 C15 175.3(2) . . . . ?
C9 N2 C6 C1 -175.4(2) . . . . ?
Ni1 N2 C6 C1 24.6(3) . . . . ?
C9 N2 C6 C7 0.7(2) . . . . ?
Ni1 N2 C6 C7 -159.25(15) . . . . ?
N2 C9 C8 C7 -0.3(3) . . . . ?
C31 C9 C8 C7 -178.0(2) . . . . ?
F5 C16 C15 F4 1.7(3) . . . . ?
C11 C16 C15 F4 -178.8(2) . . . . ?
F5 C16 C15 C14 -176.3(2) . . . . ?
C11 C16 C15 C14 3.2(4) . . . . ?
C16 C11 C12 F1 178.5(2) . . . . ?
C1 C11 C12 F1 1.5(4) . . . . ?
C16 C11 C12 C13 0.0(4) . . . . ?
C1 C11 C12 C13 -177.1(2) . . . . ?
F1 C12 C13 F2 2.1(4) . . . . ?
C11 C12 C13 F2 -179.4(2) . . . . ?
F1 C12 C13 C14 -178.2(2) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
N2 C6 C1 C2 3.6(4) . . . . ?
C7 C6 C1 C2 -171.7(2) . . . . ?
N2 C6 C1 C11 -179.71(19) . . . . ?
C7 C6 C1 C11 5.0(3) . . . . ?
C16 C11 C1 C2 -73.0(3) . . . . ?
C12 C11 C1 C2 104.0(3) . . . . ?
C16 C11 C1 C6 109.9(2) . . . . ?
C12 C11 C1 C6 -73.2(3) . . . . ?
C2 N1 C5 C4 0.7(3) . . . . ?
Ni1 N1 C5 C4 -169.18(18) . . . . ?
C2 N1 C5 C21 -175.8(2) . . . . ?
Ni1 N1 C5 C21 14.4(4) . . . . ?
C9 C31 C33 C39 -178.45(19) . . . . ?
C32 C31 C33 C39 59.3(2) . . . . ?
C34 C31 C33 C39 -58.4(2) . . . . ?
C9 C31 C32 C37 179.29(18) . . . . ?
C34 C31 C32 C37 58.2(2) . . . . ?
C33 C31 C32 C37 -59.0(2) . . . . ?
C41 N3 C45 C44 -0.4(4) . . . . ?
Ni1 N3 C45 C44 170.66(19) . . . . ?
C6 C1 C2 N1 -6.9(4) . . . . ?
C11 C1 C2 N1 176.3(2) . . . . ?
C6 C1 C2 C3 163.2(2) . . . . ?
C11 C1 C2 C3 -13.5(3) . . . . ?
C5 N1 C2 C1 169.8(2) . . . . ?
Ni1 N1 C2 C1 -17.7(3) . . . . ?
C5 N1 C2 C3 -1.7(3) . . . . ?
Ni1 N1 C2 C3 170.78(15) . . . . ?
C9 C31 C34 C35 179.41(18) . . . . ?
C32 C31 C34 C35 -58.5(2) . . . . ?
C33 C31 C34 C35 58.9(2) . . . . ?
C31 C34 C35 C36 59.3(3) . . . . ?
C31 C34 C35 C40 -60.3(3) . . . . ?
C37 C38 C39 C40 -59.3(2) . . . . ?
C37 C38 C39 C33 60.8(2) . . . . ?
C31 C33 C39 C40 59.8(2) . . . . ?
C31 C33 C39 C38 -60.5(2) . . . . ?
C9 C8 C7 C6 0.7(3) . . . . ?
N2 C6 C7 C8 -0.9(3) . . . . ?
C1 C6 C7 C8 174.9(2) . . . . ?
F2 C13 C14 F3 1.5(4) . . . . ?
C12 C13 C14 F3 -178.3(2) . . . . ?
F2 C13 C14 C15 -179.3(2) . . . . ?
C12 C13 C14 C15 0.9(4) . . . . ?
F4 C15 C14 F3 -1.5(4) . . . . ?
C16 C15 C14 F3 176.5(2) . . . . ?
F4 C15 C14 C13 179.3(2) . . . . ?
C16 C15 C14 C13 -2.7(4) . . . . ?
C39 C38 C37 C36 59.3(2) . . . . ?
C39 C38 C37 C32 -61.1(2) . . . . ?
C31 C32 C37 C36 -59.6(2) . . . . ?
C31 C32 C37 C38 60.6(2) . . . . ?
N1 C5 C4 C3 0.6(3) . . . . ?
C21 C5 C4 C3 177.0(2) . . . . ?
C38 C39 C40 C35 59.6(2) . . . . ?
C33 C39 C40 C35 -59.9(2) . . . . ?
C36 C35 C40 C39 -59.7(2) . . . . ?
C34 C35 C40 C39 59.9(3) . . . . ?
N3 C45 C44 C43 -0.7(4) . . . . ?
C5 C4 C3 C2 -1.6(3) . . . . ?
C1 C2 C3 C4 -169.4(2) . . . . ?
N1 C2 C3 C4 2.1(3) . . . . ?
C38 C37 C36 C35 -60.1(2) . . . . ?
C32 C37 C36 C35 59.9(2) . . . . ?
C40 C35 C36 C37 60.1(2) . . . . ?
C34 C35 C36 C37 -59.3(3) . . . . ?
N1 C5 C21 C22 39.6(3) . . . . ?
C4 C5 C21 C22 -136.3(3) . . . . ?
N1 C5 C21 C24 158.5(2) . . . . ?
C4 C5 C21 C24 -17.4(3) . . . . ?
N1 C5 C21 C23 -81.5(3) . . . . ?
C4 C5 C21 C23 102.6(3) . . . . ?
C5 C21 C22 C27 178.5(2) . . . . ?
C24 C21 C22 C27 58.6(3) . . . . ?
C23 C21 C22 C27 -58.3(3) . . . . ?
C5 C21 C23 C29 179.1(2) . . . . ?
C22 C21 C23 C29 57.7(3) . . . . ?
C24 C21 C23 C29 -59.6(3) . . . . ?
C45 N3 C41 C42 0.8(4) . . . . ?
Ni1 N3 C41 C42 -169.2(2) . . . . ?
C5 C21 C24 C25 -178.0(2) . . . . ?
C22 C21 C24 C25 -58.4(3) . . . . ?
C23 C21 C24 C25 59.2(3) . . . . ?
C21 C23 C29 C28 -59.4(3) . . . . ?
C21 C23 C29 C30 60.6(3) . . . . ?
C21 C22 C27 C26 -59.9(3) . . . . ?
C21 C22 C27 C28 60.3(3) . . . . ?
C25 C26 C27 C22 60.6(3) . . . . ?
C25 C26 C27 C28 -58.9(3) . . . . ?
C27 C26 C25 C30 59.8(3) . . . . ?
C27 C26 C25 C24 -60.3(3) . . . . ?
C21 C24 C25 C26 59.7(3) . . . . ?
C21 C24 C25 C30 -60.3(3) . . . . ?
C45 C44 C43 C42 1.4(4) . . . . ?
N3 C41 C42 C43 -0.2(5) . . . . ?
C44 C43 C42 C41 -0.9(5) . . . . ?
C23 C29 C28 C27 61.0(3) . . . . ?
C30 C29 C28 C27 -59.0(3) . . . . ?
C22 C27 C28 C29 -61.3(3) . . . . ?
C26 C27 C28 C29 58.4(3) . . . . ?
C26 C25 C30 C29 -60.1(3) . . . . ?
C24 C25 C30 C29 59.5(3) . . . . ?
C28 C29 C30 C25 60.0(3) . . . . ?
C23 C29 C30 C25 -59.9(3) . . . . ?
_refine_diff_density_max 0.702
_refine_diff_density_min -0.408
_refine_diff_density_rms 0.065
_shelx_res_file
;
dyy_10.res created by SHELXL-2014/7
TITL DYY_10_a.res in P2(1)/c
REM Old TITL DYY_10 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.163, Rweak 0.004, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C48 Ni
CELL 1.54178 17.7017 15.1269 13.141 90 109.571 90
ZERR 4 0.0003 0.0002 0.0002 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N Ni
UNIT 160 156 20 12 4
L.S. 10
PLAN 20
SIZE 0.08 0.21 0.42
TEMP -173.03
conf
BOND $H
LIST 4
fmap 2
acta
REM
REM
REM
WGHT 0.074100 1.381100
FVAR 0.07298
NI1 5 0.717150 0.259932 0.761493 11.00000 0.02171 0.02352 =
0.02463 -0.00003 0.00359 0.00031
F1 3 0.735573 0.628369 0.717775 11.00000 0.05669 0.03205 =
0.02838 0.00124 0.01300 -0.00765
F5 3 0.753830 0.483368 1.043173 11.00000 0.04433 0.03746 =
0.02900 0.00535 0.01210 0.00347
F4 3 0.779575 0.639079 1.146535 11.00000 0.04800 0.05348 =
0.02753 -0.00606 0.00788 0.01034
F2 3 0.752722 0.785184 0.820802 11.00000 0.05865 0.02792 =
0.04653 0.00108 0.01261 -0.00871
F3 3 0.772950 0.791826 1.033433 11.00000 0.04657 0.03629 =
0.04635 -0.01599 0.00751 -0.00367
N2 4 0.647808 0.357891 0.697557 11.00000 0.02316 0.02262 =
0.02041 0.00026 0.00391 -0.00293
N1 4 0.817904 0.329703 0.815788 11.00000 0.02203 0.03079 =
0.02532 0.00087 0.00530 -0.00136
N3 4 0.731496 0.151956 0.847892 11.00000 0.02368 0.02500 =
0.02919 -0.00077 0.00361 0.00364
C9 1 0.571417 0.360514 0.629656 11.00000 0.02278 0.02536 =
0.02029 0.00365 0.00489 -0.00076
C11 1 0.744643 0.550847 0.877529 11.00000 0.02504 0.02665 =
0.02675 -0.00213 0.00544 -0.00337
C31 1 0.535407 0.285253 0.553808 11.00000 0.02222 0.02303 =
0.02218 0.00176 0.00445 0.00013
C16 1 0.755620 0.557045 0.986544 11.00000 0.02490 0.03387 =
0.02899 0.00167 0.00656 0.00168
C6 1 0.662242 0.438775 0.752057 11.00000 0.02888 0.02249 =
0.02292 0.00079 0.00773 -0.00330
C8 1 0.535164 0.442730 0.639328 11.00000 0.02672 0.02547 =
0.02639 0.00222 0.00299 0.00431
AFIX 43
H8 2 0.481929 0.460635 0.599941 11.00000 -1.20000
AFIX 0
C15 1 0.767897 0.636369 1.041073 11.00000 0.02707 0.04227 =
0.02322 -0.00507 0.00307 0.00289
C12 1 0.744149 0.629391 0.822912 11.00000 0.03194 0.03083 =
0.02387 -0.00167 0.00679 -0.00551
C13 1 0.754166 0.710221 0.875264 11.00000 0.03075 0.02730 =
0.03684 0.00207 0.00629 -0.00399
C1 1 0.737811 0.461983 0.824200 11.00000 0.03164 0.02476 =
0.02252 0.00027 0.00900 -0.00434
C5 1 0.897288 0.315186 0.842836 11.00000 0.02263 0.04051 =
0.02902 0.00029 0.00874 -0.00173
C33 1 0.553592 0.196096 0.614355 11.00000 0.02638 0.02505 =
0.02412 0.00119 0.00447 0.00185
AFIX 23
H33A 2 0.612315 0.188648 0.647694 11.00000 -1.20000
H33B 2 0.529940 0.195804 0.672779 11.00000 -1.20000
AFIX 0
C32 1 0.443985 0.295108 0.503144 11.00000 0.02203 0.02641 =
0.02773 0.00201 0.00418 0.00157
AFIX 23
H32A 2 0.419553 0.295697 0.560776 11.00000 -1.20000
H32B 2 0.431077 0.351844 0.463531 11.00000 -1.20000
AFIX 0
C45 1 0.758846 0.162002 0.955837 11.00000 0.02958 0.03000 =
0.02889 0.00183 0.00863 0.00672
AFIX 43
H45 2 0.777242 0.218860 0.984071 11.00000 -1.20000
AFIX 0
C2 1 0.809614 0.415359 0.850285 11.00000 0.02996 0.03083 =
0.02219 -0.00043 0.00731 -0.00533
C34 1 0.572041 0.282697 0.462941 11.00000 0.02578 0.03205 =
0.02909 0.00017 0.00889 -0.00239
AFIX 23
H34A 2 0.560949 0.339245 0.422719 11.00000 -1.20000
H34B 2 0.630916 0.275741 0.494741 11.00000 -1.20000
AFIX 0
C38 1 0.427858 0.130665 0.488015 11.00000 0.02838 0.02669 =
0.03225 -0.00298 0.00723 -0.00489
AFIX 23
H38A 2 0.404066 0.131080 0.546298 11.00000 -1.20000
H38B 2 0.404301 0.080737 0.438934 11.00000 -1.20000
AFIX 0
C35 1 0.537176 0.206075 0.384961 11.00000 0.03539 0.03644 =
0.02764 -0.00641 0.01446 -0.00443
AFIX 13
H35 2 0.561448 0.205890 0.326331 11.00000 -1.20000
AFIX 0
C39 1 0.518957 0.119086 0.536629 11.00000 0.02946 0.02135 =
0.03176 0.00044 0.00536 0.00010
AFIX 13
H39 2 0.531355 0.061988 0.577200 11.00000 -1.20000
AFIX 0
C7 1 0.591637 0.491134 0.716236 11.00000 0.03364 0.02167 =
0.02730 0.00007 0.00734 0.00130
AFIX 43
H7 2 0.584837 0.548666 0.740843 11.00000 -1.20000
AFIX 0
C14 1 0.765382 0.713340 0.983622 11.00000 0.02751 0.03355 =
0.03887 -0.01186 0.00631 -0.00348
C37 1 0.409124 0.218139 0.425199 11.00000 0.02286 0.03060 =
0.02882 -0.00116 0.00168 -0.00123
AFIX 13
H37 2 0.349710 0.225424 0.392563 11.00000 -1.20000
AFIX 0
C4 1 0.941007 0.390471 0.896019 11.00000 0.02474 0.04673 =
0.03595 -0.00496 0.00836 -0.00849
AFIX 43
H4 2 0.997690 0.396597 0.922286 11.00000 -1.20000
AFIX 0
C40 1 0.556051 0.118739 0.447253 11.00000 0.03072 0.02993 =
0.03793 -0.00877 0.00936 0.00025
AFIX 23
H40A 2 0.534156 0.068788 0.397409 11.00000 -1.20000
H40B 2 0.614845 0.111019 0.479075 11.00000 -1.20000
AFIX 0
C44 1 0.761821 0.094754 1.028111 11.00000 0.03267 0.04444 =
0.03534 0.00941 0.01139 0.01358
AFIX 43
H44 2 0.782297 0.105145 1.103742 11.00000 -1.20000
AFIX 0
C3 1 0.886952 0.451972 0.902394 11.00000 0.02953 0.03562 =
0.03511 -0.00544 0.00883 -0.01145
AFIX 43
H3 2 0.898547 0.508559 0.935314 11.00000 -1.20000
AFIX 0
C36 1 0.446210 0.217188 0.335603 11.00000 0.03830 0.03331 =
0.02384 -0.00445 0.00301 -0.00601
AFIX 23
H36A 2 0.433644 0.273208 0.294395 11.00000 -1.20000
H36B 2 0.423316 0.167863 0.285180 11.00000 -1.20000
AFIX 0
C21 1 0.933591 0.232608 0.813980 11.00000 0.02296 0.04453 =
0.02996 -0.00254 0.00585 0.00307
C22 1 0.883940 0.203542 0.698364 11.00000 0.02953 0.04695 =
0.03321 -0.00507 0.00772 0.00248
AFIX 23
H22A 2 0.828278 0.190496 0.694669 11.00000 -1.20000
H22B 2 0.882193 0.252197 0.647238 11.00000 -1.20000
AFIX 0
C23 1 0.936764 0.155435 0.892382 11.00000 0.03030 0.04819 =
0.03495 0.00128 0.00530 0.00483
AFIX 23
H23A 2 0.969753 0.172736 0.966646 11.00000 -1.20000
H23B 2 0.881952 0.142082 0.892133 11.00000 -1.20000
AFIX 0
C41 1 0.706370 0.070943 0.810444 11.00000 0.04764 0.02860 =
0.04263 -0.00096 -0.00437 0.00460
AFIX 43
H41 2 0.687433 0.061776 0.734540 11.00000 -1.20000
AFIX 0
C24 1 1.020246 0.251503 0.817609 11.00000 0.02388 0.05911 =
0.03852 -0.00501 0.00703 0.00076
AFIX 23
H24A 2 1.020042 0.300828 0.768002 11.00000 -1.20000
H24B 2 1.053265 0.269465 0.891599 11.00000 -1.20000
AFIX 0
C29 1 0.972795 0.072927 0.858634 11.00000 0.04462 0.04580 =
0.05496 0.00560 0.01046 0.01458
AFIX 13
H29 2 0.973899 0.023384 0.909496 11.00000 -1.20000
AFIX 0
C26 1 1.006231 0.142525 0.670559 11.00000 0.03774 0.06371 =
0.05306 -0.01268 0.01749 0.01036
AFIX 23
H26A 2 1.030012 0.090006 0.647979 11.00000 -1.20000
H26B 2 1.005321 0.191395 0.620053 11.00000 -1.20000
AFIX 0
C27 1 0.920722 0.121453 0.665951 11.00000 0.03699 0.05703 =
0.04020 -0.01336 0.00954 0.00600
AFIX 13
H27 2 0.887968 0.103575 0.590846 11.00000 -1.20000
AFIX 0
C25 1 1.057012 0.168930 0.784484 11.00000 0.02648 0.07025 =
0.05503 -0.00796 0.01208 0.00776
AFIX 13
H25 2 1.112809 0.182459 0.786576 11.00000 -1.20000
AFIX 0
C43 1 0.734600 0.012727 0.988364 11.00000 0.04601 0.03852 =
0.05883 0.02257 0.01013 0.00742
AFIX 43
H43 2 0.734777 -0.034612 1.035949 11.00000 -1.20000
AFIX 0
C42 1 0.706685 -0.000063 0.877094 11.00000 0.05804 0.02363 =
0.06899 0.00827 -0.00631 -0.00224
AFIX 43
H42 2 0.688176 -0.056482 0.847379 11.00000 -1.20000
AFIX 0
C28 1 0.921458 0.046455 0.744186 11.00000 0.03931 0.04461 =
0.06117 -0.01190 0.01243 0.01045
AFIX 23
H28A 2 0.866032 0.033793 0.741856 11.00000 -1.20000
H28B 2 0.943507 -0.007782 0.722600 11.00000 -1.20000
AFIX 0
C30 1 1.058977 0.093313 0.861857 11.00000 0.03555 0.06308 =
0.06014 -0.00571 0.00326 0.01943
AFIX 23
H30A 2 1.092527 0.109957 0.936116 11.00000 -1.20000
H30B 2 1.082718 0.040135 0.840626 11.00000 -1.20000
AFIX 0
HKLF 4
REM DYY_10_a.res in P2(1)/c
REM R1 = 0.0444 for 4658 Fo > 4sig(Fo) and 0.0558 for all 5677 data
REM 442 parameters refined using 0 restraints
END
WGHT 0.0741 1.3876
REM Highest difference peak 0.702, deepest hole -0.408, 1-sigma level 0.065
Q1 1 0.7292 0.2597 0.6871 11.00000 0.05 0.70
Q2 1 0.6906 0.2616 0.8250 11.00000 0.05 0.66
Q3 1 0.5469 0.2828 0.5074 11.00000 0.05 0.35
Q4 1 0.7740 0.7141 0.9163 11.00000 0.05 0.33
Q5 1 0.7608 0.5801 0.8520 11.00000 0.05 0.33
Q6 1 0.5410 0.2432 0.5781 11.00000 0.05 0.31
Q7 1 0.7727 0.7803 0.7572 11.00000 0.05 0.31
Q8 1 0.7779 0.6776 0.8581 11.00000 0.05 0.30
Q9 1 0.5309 0.1574 0.5688 11.00000 0.05 0.30
Q10 1 0.7764 0.7199 0.8193 11.00000 0.05 0.28
Q11 1 0.5412 0.1581 0.4196 11.00000 0.05 0.28
Q12 1 0.7322 0.0185 0.8409 11.00000 0.05 0.28
Q13 1 0.7662 0.6267 0.7814 11.00000 0.05 0.28
Q14 1 0.7398 -0.0035 0.9359 11.00000 0.05 0.27
Q15 1 0.5500 0.3154 0.5918 11.00000 0.05 0.27
Q16 1 0.5603 0.4028 0.6178 11.00000 0.05 0.27
Q17 1 0.9099 0.2154 0.7629 11.00000 0.05 0.27
Q18 1 0.7186 0.0684 0.7468 11.00000 0.05 0.26
Q19 1 0.5319 0.0994 0.4664 11.00000 0.05 0.26
Q20 1 0.4298 0.2182 0.3836 11.00000 0.05 0.26
;
_shelx_res_checksum 98051