# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2021
#######################################################################
#
# 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_ms2k_c1
_database_code_depnum_ccdc_archive 'CCDC 1956236'
loop_
_audit_author_name
_audit_author_address
'Dan G Dumitrescu'
;Sincrotrone Elettra Trieste
Italy
;
_audit_update_record
;
2019-09-26 deposited with the CCDC. 2021-02-01 downloaded from the CCDC.
;
_audit_creation_date 2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C15 H16 N6 O P), 2(C15 H15 N6 O P), H2 O'
_chemical_formula_sum 'C60 H64 N24 O5 P4'
_chemical_formula_weight 1325.23
_chemical_melting_point ?
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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.568(2)
_cell_length_b 13.475(3)
_cell_length_c 21.853(4)
_cell_angle_alpha 90
_cell_angle_beta 92.35(3)
_cell_angle_gamma 90
_cell_volume 3109.3(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 33356
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.672
_cell_measurement_theta_min 1.749
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.969
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.416
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1817
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0246
_diffrn_reflns_av_unetI/netI 0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 44499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 24.835
_diffrn_reflns_theta_max 27.672
_diffrn_reflns_theta_min 1.749
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Arinax MD2S/Pilatus 6M'
_diffrn_measurement_method 'rotating crystal'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.700
_diffrn_source SCW
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7346
_reflns_number_total 7572
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.292
_refine_diff_density_min -0.465
_refine_diff_density_rms 0.069
_refine_ls_extinction_coef 0.0610(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 570
_refine_ls_number_reflns 7572
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0359
_refine_ls_R_factor_gt 0.0354
_refine_ls_restrained_S_all 1.043
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+1.1480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0941
_refine_ls_wR_factor_ref 0.0947
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.5 times of:
All O(H,H) groups
2. Restrained distances
C1-H1
0.98 with sigma of 0.02
C0-H0
0.98 with sigma of 0.02
3. Others
Fixed Sof: C0(0.5) N0(0.5) O1(0.5) H1A(0.5) H1B(0.5) N0AA(0.5) C1(0.5)
4.a Free rotating group:
O1(H1A,H1B)
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
P001 P 0.68242(3) 0.30916(2) 0.37617(2) 0.01961(8) Uani 1 1 d . . . . .
P002 P 0.54076(2) 0.55074(2) 0.25417(2) 0.01821(8) Uani 1 1 d . . . . .
O003 O 0.47490(7) 0.45540(5) 0.26398(4) 0.02287(17) Uani 1 1 d . . . . .
O004 O 0.65867(8) 0.41264(6) 0.39583(4) 0.02544(17) Uani 1 1 d . . . . .
N005 N 0.58193(9) 0.60268(7) 0.08128(4) 0.02267(19) Uani 1 1 d . . . . .
N006 N 0.62221(9) 0.10599(7) 0.32183(4) 0.02115(18) Uani 1 1 d . . . . .
N007 N 0.73255(9) 0.71969(7) 0.28435(4) 0.02002(18) Uani 1 1 d . . . . .
N008 N 0.69095(9) 0.22720(7) 0.43201(4) 0.02058(18) Uani 1 1 d . . . . .
N009 N 0.45133(9) 0.64914(7) 0.26315(4) 0.02124(18) Uani 1 1 d . . . . .
N00A N 0.81951(9) 0.29606(7) 0.34290(4) 0.02057(18) Uani 1 1 d . . . . .
N00B N 0.66805(9) 0.55513(7) 0.30085(4) 0.02095(18) Uani 1 1 d . . . . .
N00C N 0.57266(9) 0.27528(7) 0.32454(4) 0.02105(18) Uani 1 1 d . . . . .
N00D N 0.59503(9) 0.56714(7) 0.18475(4) 0.01979(18) Uani 1 1 d . . . . .
N00E N 1.03468(9) 0.30366(7) 0.33118(5) 0.0246(2) Uani 1 1 d . . . . .
N00F N 0.31439(10) 0.75564(8) 0.30868(5) 0.0316(2) Uani 1 1 d . . . . .
C0 C 0.6203(12) 0.1158(10) 0.5058(7) 0.0223(13) Uani 0.5 1 d D . P A 2
C00H C 0.93844(10) 0.32579(7) 0.36648(5) 0.0211(2) Uani 1 1 d . . . . .
C00I C 0.52015(10) 0.57463(7) 0.13052(5) 0.0199(2) Uani 1 1 d . . . . .
C00J C 0.53937(10) 0.17827(8) 0.30741(5) 0.0196(2) Uani 1 1 d . . . . .
C00K C 0.73997(10) 0.63776(7) 0.31888(5) 0.01946(19) Uani 1 1 d . . . . .
C00L C 0.95577(12) 0.37538(9) 0.42290(5) 0.0268(2) Uani 1 1 d . . . . .
C00M C 0.37918(10) 0.67062(8) 0.31382(5) 0.0240(2) Uani 1 1 d . . . . .
C00N C 0.59413(10) 0.20554(8) 0.47193(5) 0.0213(2) Uani 1 1 d . . . . .
C00O C 0.80448(10) 0.79778(8) 0.30293(5) 0.0215(2) Uani 1 1 d . . . . .
N0 N 0.5012(10) 0.2680(7) 0.4768(4) 0.040(2) Uani 0.5 1 d . . P A 2
C00Q C 0.58580(10) 0.01223(8) 0.30869(5) 0.0230(2) Uani 1 1 d . . . . .
C00R C 0.51348(12) 0.61507(9) 0.02849(5) 0.0280(2) Uani 1 1 d . . . . .
C00S C 0.81829(11) 0.63044(8) 0.37231(5) 0.0250(2) Uani 1 1 d . . . . .
C00T C 0.38963(11) 0.55473(9) 0.12855(6) 0.0274(2) Uani 1 1 d . . . . .
C00U C 0.42312(11) 0.16071(9) 0.27640(5) 0.0276(2) Uani 1 1 d . . . . .
C00V C 0.89088(12) 0.71143(9) 0.38993(6) 0.0287(2) Uani 1 1 d . . . . .
C00W C 0.47175(11) -0.01315(9) 0.27977(6) 0.0276(2) Uani 1 1 d . . . . .
C00X C 1.15198(12) 0.33177(9) 0.35038(7) 0.0319(3) Uani 1 1 d . . . . .
C00Y C 0.38441(13) 0.60118(10) 0.02253(6) 0.0332(3) Uani 1 1 d . . . . .
C00Z C 0.37622(14) 0.60815(10) 0.36494(6) 0.0340(3) Uani 1 1 d . . . . .
C010 C 0.88431(11) 0.79782(8) 0.35455(5) 0.0255(2) Uani 1 1 d . . . . .
C011 C 1.07744(13) 0.40264(9) 0.44154(6) 0.0321(3) Uani 1 1 d . . . . .
C012 C 0.38987(12) 0.06390(10) 0.26239(6) 0.0323(3) Uani 1 1 d . . . . .
C013 C 0.32190(12) 0.56957(11) 0.07371(6) 0.0346(3) Uani 1 1 d . . . . .
C014 C 1.17812(13) 0.38104(10) 0.40488(7) 0.0343(3) Uani 1 1 d . . . . .
C015 C 0.41985(13) 0.16455(14) 0.55653(7) 0.0419(3) Uani 1 1 d . . . . .
C016 C 0.40693(14) 0.24739(14) 0.51974(7) 0.0444(4) Uani 1 1 d . . . . .
C017 C 0.52106(14) 0.10243(12) 0.54754(7) 0.0400(3) Uani 1 1 d . . . . .
C018 C 0.30075(16) 0.63593(13) 0.41241(7) 0.0451(4) Uani 1 1 d . . . . .
C019 C 0.24209(14) 0.77960(13) 0.35587(8) 0.0454(4) Uani 1 1 d . . . . .
C01A C 0.23191(15) 0.72263(14) 0.40779(8) 0.0493(4) Uani 1 1 d . . . . .
O1 O 0.6005(8) 0.5205(4) 0.4990(3) 0.165(3) Uani 0.5 1 d . . P . .
H1A H 0.563099 0.566560 0.478866 0.248 Uiso 0.5 1 d G . P . .
H1B H 0.617512 0.473129 0.475004 0.248 Uiso 0.5 1 d G . P . .
H00L H 0.8858(16) 0.3895(12) 0.4479(8) 0.035(4) Uiso 1 1 d . . . . .
H00O H 0.7973(14) 0.8544(11) 0.2766(7) 0.024(3) Uiso 1 1 d . . . . .
H00R H 0.5627(16) 0.6348(13) -0.0078(8) 0.039(4) Uiso 1 1 d . . . . .
H00T H 0.3497(16) 0.5344(13) 0.1645(8) 0.038(4) Uiso 1 1 d . . . . .
H00V H 0.9472(16) 0.7068(14) 0.4264(8) 0.040(4) Uiso 1 1 d . . . . .
H00Y H 0.3434(18) 0.6112(14) -0.0150(9) 0.048(5) Uiso 1 1 d . . . . .
H00S H 0.8179(14) 0.5690(12) 0.3956(7) 0.028(4) Uiso 1 1 d . . . . .
H008 H 0.7463(15) 0.1791(12) 0.4276(7) 0.032(4) Uiso 1 1 d . . . . .
H011 H 1.0883(16) 0.4382(13) 0.4812(8) 0.041(5) Uiso 1 1 d . . . . .
H010 H 0.9348(16) 0.8575(13) 0.3653(8) 0.037(4) Uiso 1 1 d . . . . .
H00X H 1.2207(17) 0.3144(13) 0.3209(8) 0.043(5) Uiso 1 1 d . . . . .
H00A H 0.8195(16) 0.2679(13) 0.3070(8) 0.036(4) Uiso 1 1 d . . . . .
H00D H 0.6750(16) 0.5839(13) 0.1816(7) 0.032(4) Uiso 1 1 d . . . . .
H013 H 0.2293(18) 0.5591(14) 0.0725(9) 0.046(5) Uiso 1 1 d . . . . .
H00Q H 0.6459(15) -0.0381(13) 0.3199(7) 0.033(4) Uiso 1 1 d . . . . .
H019 H 0.196(2) 0.8372(17) 0.3501(10) 0.058(6) Uiso 1 1 d . . . . .
H015 H 0.362(2) 0.1487(16) 0.5877(10) 0.058(6) Uiso 1 1 d . . . . .
H00Z H 0.4284(18) 0.5470(14) 0.3670(9) 0.046(5) Uiso 1 1 d . . . . .
H018 H 0.296(2) 0.5954(16) 0.4482(10) 0.062(6) Uiso 1 1 d . . . . .
H00B H 0.6687(16) 0.5095(14) 0.3269(8) 0.037(4) Uiso 1 1 d . . . . .
H00W H 0.4493(15) -0.0815(13) 0.2725(7) 0.032(4) Uiso 1 1 d . . . . .
H00U H 0.3694(17) 0.2160(14) 0.2662(8) 0.039(4) Uiso 1 1 d . . . . .
H016 H 0.341(2) 0.2920(16) 0.5246(9) 0.056(6) Uiso 1 1 d . . . . .
H009 H 0.4597(17) 0.6947(14) 0.2391(8) 0.039(4) Uiso 1 1 d . . . . .
H012 H 0.3074(17) 0.0496(13) 0.2421(8) 0.041(5) Uiso 1 1 d . . . . .
H01A H 0.176(2) 0.7422(16) 0.4393(10) 0.061(6) Uiso 1 1 d . . . . .
H017 H 0.5316(19) 0.0408(16) 0.5719(9) 0.052(5) Uiso 1 1 d . . . . .
H00C H 0.5347(16) 0.3237(14) 0.3066(8) 0.037(4) Uiso 1 1 d . . . . .
N0AA N 0.5992(10) 0.1268(9) 0.5049(6) 0.0232(16) Uani 0.5 1 d . . P A 1
C1 C 0.4882(11) 0.2688(7) 0.4776(6) 0.0301(19) Uani 0.5 1 d D . P A 1
H014 H 1.2614(19) 0.3975(14) 0.4173(9) 0.049(5) Uiso 1 1 d . . . . .
H1 H 0.477(3) 0.3244(18) 0.4476(11) 0.091(8) Uiso 1 1 d D . . . .
H0 H 0.682(3) 0.071(3) 0.491(2) 0.179(17) Uiso 1 1 d 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
P001 0.02431(14) 0.01536(14) 0.01921(14) 0.00230(9) 0.00155(10) 0.00002(9)
P002 0.02055(14) 0.01325(13) 0.02080(14) 0.00004(9) 0.00056(9) 0.00026(8)
O003 0.0254(4) 0.0157(3) 0.0273(4) 0.0010(3) -0.0001(3) -0.0022(3)
O004 0.0346(4) 0.0172(4) 0.0247(4) 0.0011(3) 0.0033(3) 0.0012(3)
N005 0.0268(4) 0.0185(4) 0.0226(4) -0.0016(3) 0.0004(3) -0.0014(3)
N006 0.0214(4) 0.0174(4) 0.0246(4) 0.0035(3) 0.0003(3) 0.0004(3)
N007 0.0239(4) 0.0160(4) 0.0203(4) -0.0002(3) 0.0026(3) 0.0004(3)
N008 0.0236(4) 0.0183(4) 0.0200(4) 0.0030(3) 0.0027(3) 0.0021(3)
N009 0.0235(4) 0.0154(4) 0.0251(4) 0.0004(3) 0.0039(3) 0.0016(3)
N00A 0.0242(4) 0.0190(4) 0.0186(4) -0.0003(3) 0.0012(3) -0.0031(3)
N00B 0.0256(4) 0.0146(4) 0.0224(4) 0.0023(3) -0.0026(3) -0.0011(3)
N00C 0.0246(4) 0.0159(4) 0.0225(4) 0.0036(3) -0.0007(3) 0.0021(3)
N00D 0.0195(4) 0.0185(4) 0.0213(4) -0.0009(3) 0.0004(3) -0.0002(3)
N00E 0.0251(5) 0.0188(4) 0.0300(5) -0.0011(3) 0.0003(4) -0.0018(3)
N00F 0.0232(5) 0.0287(5) 0.0428(6) -0.0145(4) -0.0007(4) 0.0022(4)
C0 0.017(4) 0.024(2) 0.0269(18) 0.0155(15) 0.005(2) 0.010(2)
C00H 0.0259(5) 0.0141(4) 0.0231(5) 0.0030(4) -0.0011(4) -0.0018(4)
C00I 0.0238(5) 0.0132(4) 0.0225(5) -0.0019(3) -0.0013(4) 0.0000(4)
C00J 0.0216(5) 0.0187(5) 0.0187(4) 0.0016(4) 0.0023(4) 0.0013(4)
C00K 0.0214(5) 0.0160(4) 0.0211(5) -0.0011(4) 0.0023(4) 0.0002(3)
C00L 0.0345(6) 0.0210(5) 0.0246(5) -0.0003(4) -0.0020(4) -0.0030(4)
C00M 0.0206(5) 0.0221(5) 0.0294(5) -0.0092(4) 0.0028(4) -0.0047(4)
C00N 0.0223(5) 0.0239(5) 0.0177(4) 0.0017(4) 0.0000(4) -0.0012(4)
C00O 0.0267(5) 0.0158(4) 0.0225(5) -0.0011(4) 0.0057(4) 0.0001(4)
N0 0.044(4) 0.052(4) 0.025(3) 0.016(2) 0.012(2) -0.001(3)
C00Q 0.0254(5) 0.0182(5) 0.0255(5) 0.0021(4) 0.0016(4) 0.0007(4)
C00R 0.0358(6) 0.0244(5) 0.0237(5) 0.0013(4) -0.0015(4) -0.0042(4)
C00S 0.0300(5) 0.0203(5) 0.0244(5) 0.0027(4) -0.0031(4) -0.0019(4)
C00T 0.0255(5) 0.0282(6) 0.0282(6) 0.0019(4) -0.0014(4) -0.0063(4)
C00U 0.0250(5) 0.0272(6) 0.0301(6) -0.0038(4) -0.0047(4) 0.0065(4)
C00V 0.0326(6) 0.0264(5) 0.0265(5) 0.0003(4) -0.0057(4) -0.0045(5)
C00W 0.0292(6) 0.0227(5) 0.0308(6) -0.0042(4) 0.0009(4) -0.0031(4)
C00X 0.0259(6) 0.0259(6) 0.0438(7) -0.0029(5) -0.0011(5) -0.0026(4)
C00Y 0.0370(6) 0.0325(6) 0.0290(6) 0.0041(5) -0.0103(5) -0.0050(5)
C00Z 0.0416(7) 0.0299(6) 0.0313(6) -0.0064(5) 0.0118(5) -0.0083(5)
C010 0.0291(5) 0.0206(5) 0.0268(5) -0.0036(4) 0.0018(4) -0.0054(4)
C011 0.0408(7) 0.0230(5) 0.0316(6) -0.0020(5) -0.0097(5) -0.0040(5)
C012 0.0255(6) 0.0333(6) 0.0374(6) -0.0091(5) -0.0066(5) 0.0005(5)
C013 0.0274(6) 0.0388(7) 0.0367(7) 0.0032(5) -0.0076(5) -0.0080(5)
C014 0.0300(6) 0.0261(6) 0.0460(7) -0.0014(5) -0.0101(5) -0.0049(5)
C015 0.0275(6) 0.0661(10) 0.0325(6) 0.0189(7) 0.0075(5) 0.0011(6)
C016 0.0355(7) 0.0626(10) 0.0357(7) 0.0141(7) 0.0092(6) 0.0147(7)
C017 0.0354(7) 0.0511(8) 0.0338(6) 0.0193(6) 0.0058(5) 0.0010(6)
C018 0.0518(9) 0.0482(8) 0.0365(7) -0.0164(6) 0.0190(6) -0.0211(7)
C019 0.0296(6) 0.0469(8) 0.0599(9) -0.0294(7) 0.0054(6) 0.0043(6)
C01A 0.0377(7) 0.0615(10) 0.0500(9) -0.0328(8) 0.0192(6) -0.0129(7)
O1 0.296(8) 0.070(3) 0.122(4) -0.036(3) -0.083(5) 0.071(4)
N0AA 0.014(3) 0.028(3) 0.0281(16) 0.0062(17) 0.0007(17) 0.0112(19)
C1 0.0223(19) 0.031(3) 0.038(4) 0.006(2) 0.0043(18) 0.019(2)
_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
P001 O004 1.4836(9) . ?
P001 N008 1.6455(9) . ?
P001 N00A 1.6568(10) . ?
P001 N00C 1.6491(11) . ?
P002 O003 1.4809(8) . ?
P002 N009 1.6447(10) . ?
P002 N00B 1.6557(11) . ?
P002 N00D 1.6585(10) . ?
N005 C00I 1.3360(14) . ?
N005 C00R 1.3467(15) . ?
N006 C00J 1.3386(13) . ?
N006 C00Q 1.3483(14) . ?
N007 C00K 1.3378(13) . ?
N007 C00O 1.3507(14) . ?
N008 C00N 1.4022(14) . ?
N008 H008 0.881(17) . ?
N009 C00M 1.4001(14) . ?
N009 H009 0.815(19) . ?
N00A C00H 1.3974(14) . ?
N00A H00A 0.870(18) . ?
N00B C00K 1.3957(13) . ?
N00B H00B 0.838(18) . ?
N00C C00J 1.4008(14) . ?
N00C H00C 0.853(18) . ?
N00D C00I 1.4012(14) . ?
N00D H00D 0.880(17) . ?
N00E C00H 1.3352(15) . ?
N00E C00X 1.3467(15) . ?
N00F C00M 1.3370(15) . ?
N00F C019 1.3476(18) . ?
C0 C00N 1.439(12) . ?
C0 C017 1.429(12) . ?
C0 H0 0.958(19) . ?
C00H C00L 1.4077(15) . ?
C00I C00T 1.4041(15) . ?
C00J C00U 1.3987(15) . ?
C00K C00S 1.4067(15) . ?
C00L C011 1.3825(18) . ?
C00L H00L 0.956(17) . ?
C00M C00Z 1.4002(18) . ?
C00N N0 1.301(9) . ?
C00N N0AA 1.282(11) . ?
C00N C1 1.417(8) . ?
C00O C010 1.3807(17) . ?
C00O H00O 0.956(15) . ?
N0 C016 1.424(10) . ?
N0 H1 1.02(2) . ?
C00Q C00W 1.3807(16) . ?
C00Q H00Q 0.954(17) . ?
C00R C00Y 1.3777(18) . ?
C00R H00R 1.002(17) . ?
C00S C00V 1.3797(16) . ?
C00S H00S 0.972(16) . ?
C00T C013 1.3850(17) . ?
C00T H00T 0.948(17) . ?
C00U C012 1.3821(18) . ?
C00U H00U 0.958(18) . ?
C00V C010 1.3976(17) . ?
C00V H00V 0.977(18) . ?
C00W C012 1.3943(18) . ?
C00W H00W 0.963(17) . ?
C00X C014 1.3814(19) . ?
C00X H00X 1.017(19) . ?
C00Y C013 1.3889(19) . ?
C00Y H00Y 0.921(19) . ?
C00Z C018 1.3856(18) . ?
C00Z H00Z 0.992(19) . ?
C010 H010 0.987(18) . ?
C011 C014 1.389(2) . ?
C011 H011 0.992(18) . ?
C012 H012 0.981(18) . ?
C013 H013 0.989(19) . ?
C014 H014 0.94(2) . ?
C015 C016 1.379(2) . ?
C015 C017 1.379(2) . ?
C015 H015 0.96(2) . ?
C016 H016 0.93(2) . ?
C016 C1 1.317(12) . ?
C017 H017 0.99(2) . ?
C017 N0AA 1.311(11) . ?
C018 C01A 1.378(3) . ?
C018 H018 0.96(2) . ?
C019 C01A 1.378(3) . ?
C019 H019 0.92(2) . ?
C01A H01A 0.96(2) . ?
O1 H1A 0.8499 . ?
O1 H1B 0.8500 . ?
N0AA H0 1.20(3) . ?
C1 H1 0.998(17) . ?
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
O004 P001 N008 114.89(5) . . ?
O004 P001 N00A 112.87(5) . . ?
O004 P001 N00C 109.62(5) . . ?
N008 P001 N00A 103.39(5) . . ?
N008 P001 N00C 109.70(5) . . ?
N00C P001 N00A 105.87(5) . . ?
O003 P002 N009 113.97(5) . . ?
O003 P002 N00B 108.45(5) . . ?
O003 P002 N00D 115.49(5) . . ?
N009 P002 N00B 110.73(5) . . ?
N009 P002 N00D 102.93(5) . . ?
N00B P002 N00D 104.84(5) . . ?
C00I N005 C00R 117.52(10) . . ?
C00J N006 C00Q 116.96(10) . . ?
C00K N007 C00O 117.01(9) . . ?
P001 N008 H008 115.5(11) . . ?
C00N N008 P001 125.58(8) . . ?
C00N N008 H008 114.8(11) . . ?
P002 N009 H009 116.9(13) . . ?
C00M N009 P002 126.53(8) . . ?
C00M N009 H009 115.5(13) . . ?
P001 N00A H00A 118.3(11) . . ?
C00H N00A P001 126.67(8) . . ?
C00H N00A H00A 115.1(11) . . ?
P002 N00B H00B 112.1(12) . . ?
C00K N00B P002 128.45(8) . . ?
C00K N00B H00B 113.9(12) . . ?
P001 N00C H00C 114.0(12) . . ?
C00J N00C P001 127.09(7) . . ?
C00J N00C H00C 118.9(12) . . ?
P002 N00D H00D 118.3(11) . . ?
C00I N00D P002 125.35(8) . . ?
C00I N00D H00D 115.3(11) . . ?
C00H N00E C00X 118.05(11) . . ?
C00M N00F C019 116.46(13) . . ?
C00N C0 H0 118(3) . . ?
C017 C0 C00N 107.7(8) . . ?
C017 C0 H0 132(3) . . ?
N00A C00H C00L 122.80(10) . . ?
N00E C00H N00A 114.70(10) . . ?
N00E C00H C00L 122.50(11) . . ?
N005 C00I N00D 115.08(9) . . ?
N005 C00I C00T 122.77(10) . . ?
N00D C00I C00T 122.16(10) . . ?
N006 C00J N00C 117.48(9) . . ?
N006 C00J C00U 122.96(10) . . ?
C00U C00J N00C 119.56(10) . . ?
N007 C00K N00B 118.71(10) . . ?
N007 C00K C00S 123.02(10) . . ?
N00B C00K C00S 118.26(9) . . ?
C00H C00L H00L 121.2(10) . . ?
C011 C00L C00H 118.05(12) . . ?
C011 C00L H00L 120.7(10) . . ?
N009 C00M C00Z 122.51(11) . . ?
N00F C00M N009 113.85(11) . . ?
N00F C00M C00Z 123.64(11) . . ?
N008 C00N C0 111.4(5) . . ?
N008 C00N C1 121.9(5) . . ?
N0 C00N N008 119.2(4) . . ?
N0 C00N C0 129.1(6) . . ?
N0AA C00N N008 120.5(4) . . ?
N0AA C00N C1 117.6(7) . . ?
N007 C00O C010 124.29(10) . . ?
N007 C00O H00O 114.2(9) . . ?
C010 C00O H00O 121.5(9) . . ?
C00N N0 C016 118.6(6) . . ?
C00N N0 H1 127.1(18) . . ?
C016 N0 H1 113.2(18) . . ?
N006 C00Q C00W 124.46(10) . . ?
N006 C00Q H00Q 115.4(10) . . ?
C00W C00Q H00Q 120.1(10) . . ?
N005 C00R C00Y 124.00(12) . . ?
N005 C00R H00R 115.6(10) . . ?
C00Y C00R H00R 120.4(10) . . ?
C00K C00S H00S 118.7(9) . . ?
C00V C00S C00K 118.54(10) . . ?
C00V C00S H00S 122.8(9) . . ?
C00I C00T H00T 120.0(10) . . ?
C013 C00T C00I 118.11(11) . . ?
C013 C00T H00T 121.9(10) . . ?
C00J C00U H00U 118.9(11) . . ?
C012 C00U C00J 118.50(11) . . ?
C012 C00U H00U 122.6(11) . . ?
C00S C00V C010 119.34(11) . . ?
C00S C00V H00V 119.4(11) . . ?
C010 C00V H00V 121.3(11) . . ?
C00Q C00W C012 117.42(11) . . ?
C00Q C00W H00W 121.1(10) . . ?
C012 C00W H00W 121.4(10) . . ?
N00E C00X C014 123.57(12) . . ?
N00E C00X H00X 114.2(10) . . ?
C014 C00X H00X 122.2(10) . . ?
C00R C00Y C013 117.86(11) . . ?
C00R C00Y H00Y 119.4(12) . . ?
C013 C00Y H00Y 122.7(12) . . ?
C00M C00Z H00Z 120.4(11) . . ?
C018 C00Z C00M 117.85(14) . . ?
C018 C00Z H00Z 121.8(11) . . ?
C00O C010 C00V 117.80(10) . . ?
C00O C010 H010 120.0(10) . . ?
C00V C010 H010 122.2(10) . . ?
C00L C011 C014 119.97(12) . . ?
C00L C011 H011 117.3(10) . . ?
C014 C011 H011 122.8(10) . . ?
C00U C012 C00W 119.55(11) . . ?
C00U C012 H012 120.0(10) . . ?
C00W C012 H012 120.4(10) . . ?
C00T C013 C00Y 119.68(12) . . ?
C00T C013 H013 118.6(11) . . ?
C00Y C013 H013 121.7(11) . . ?
C00X C014 C011 117.85(12) . . ?
C00X C014 H014 121.0(12) . . ?
C011 C014 H014 121.1(12) . . ?
C016 C015 H015 123.0(13) . . ?
C017 C015 C016 117.85(13) . . ?
C017 C015 H015 119.2(13) . . ?
N0 C016 H016 119.9(13) . . ?
C015 C016 N0 119.1(4) . . ?
C015 C016 H016 120.8(13) . . ?
C1 C016 C015 122.2(4) . . ?
C1 C016 H016 116.9(13) . . ?
C0 C017 H017 112.3(13) . . ?
C015 C017 C0 127.5(5) . . ?
C015 C017 H017 120.2(12) . . ?
N0AA C017 C015 117.6(4) . . ?
N0AA C017 H017 122.1(12) . . ?
C00Z C018 H018 120.4(13) . . ?
C01A C018 C00Z 119.52(16) . . ?
C01A C018 H018 120.1(13) . . ?
N00F C019 C01A 124.23(15) . . ?
N00F C019 H019 114.1(14) . . ?
C01A C019 H019 121.7(13) . . ?
C018 C01A H01A 121.1(13) . . ?
C019 C01A C018 118.29(13) . . ?
C019 C01A H01A 120.6(13) . . ?
H1A O1 H1B 109.5 . . ?
C00N N0AA C017 126.4(8) . . ?
C00N N0AA H0 113(2) . . ?
C017 N0AA H0 121(2) . . ?
C00N C1 H1 117.9(19) . . ?
C016 C1 C00N 118.0(7) . . ?
C016 C1 H1 124.0(17) . . ?
_iucr_refine_instructions_details
;
TITL ms2k_c1_a.res in P2(1)/n
ms2k_c1.res
created by SHELXL-2018/1 at 18:16:06 on 26-Jun-2019
REM Old TITL ms2k_c1_a.res in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.126, Rweak 0.004, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C32 N10 O2 P2
CELL 0.7 10.568 13.475 21.853 90 92.348 90
ZERR 23 0.0021 0.0027 0.0044 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O P Cl Mn
DISP C 0.0033 0.0016 11.1819
DISP Cl 0.1453 0.1556 651.6741
DISP H -0 0 0.6234
DISP Mn 0.3441 0.7121 2905.5343
DISP N 0.0063 0.0031 18.9823
DISP O 0.0112 0.0059 31.3712
DISP P 0.1018 0.0938 394.0833
UNIT 23 23 23 23 23 23 23
DFIX 0.98 C1 H1
DFIX 0.98 C0 H0
L.S. 40
PLAN 20
FREE N0AA H0
FREE N0 H1
BOND $H
list 4
fmap 2
ACTA
REM
REM
REM
WGHT 0.055100 1.148000
EXTI 0.061035
FVAR 0.60388
P001 5 0.682424 0.309159 0.376169 11.00000 0.02431 0.01536 =
0.01921 0.00230 0.00155 0.00002
P002 5 0.540756 0.550742 0.254166 11.00000 0.02055 0.01325 =
0.02080 0.00004 0.00056 0.00026
O003 4 0.474902 0.455398 0.263984 11.00000 0.02543 0.01574 =
0.02734 0.00096 -0.00008 -0.00224
O004 4 0.658671 0.412643 0.395834 11.00000 0.03462 0.01719 =
0.02468 0.00106 0.00332 0.00118
N005 3 0.581935 0.602678 0.081278 11.00000 0.02681 0.01852 =
0.02261 -0.00164 0.00036 -0.00135
N006 3 0.622213 0.105987 0.321833 11.00000 0.02142 0.01739 =
0.02458 0.00349 0.00030 0.00035
N007 3 0.732553 0.719691 0.284354 11.00000 0.02394 0.01599 =
0.02027 -0.00025 0.00260 0.00043
N008 3 0.690949 0.227199 0.432008 11.00000 0.02362 0.01831 =
0.01997 0.00302 0.00275 0.00211
N009 3 0.451327 0.649136 0.263152 11.00000 0.02345 0.01542 =
0.02509 0.00041 0.00387 0.00157
N00A 3 0.819513 0.296060 0.342900 11.00000 0.02417 0.01900 =
0.01856 -0.00033 0.00119 -0.00313
N00B 3 0.668054 0.555132 0.300847 11.00000 0.02555 0.01461 =
0.02240 0.00230 -0.00256 -0.00110
N00C 3 0.572662 0.275284 0.324544 11.00000 0.02458 0.01591 =
0.02252 0.00361 -0.00072 0.00214
N00D 3 0.595031 0.567145 0.184745 11.00000 0.01954 0.01851 =
0.02130 -0.00090 0.00043 -0.00019
N00E 3 1.034681 0.303655 0.331176 11.00000 0.02505 0.01877 =
0.03005 -0.00108 0.00033 -0.00184
N00F 3 0.314394 0.755638 0.308679 11.00000 0.02323 0.02871 =
0.04281 -0.01451 -0.00066 0.00219
PART 2
C0 1 0.620284 0.115821 0.505826 10.50000 0.01664 0.02361 =
0.02690 0.01545 0.00500 0.01004
PART 0
C00H 1 0.938444 0.325793 0.366476 11.00000 0.02592 0.01412 =
0.02308 0.00304 -0.00112 -0.00176
C00I 1 0.520154 0.574628 0.130524 11.00000 0.02378 0.01323 =
0.02254 -0.00193 -0.00127 -0.00004
C00J 1 0.539372 0.178266 0.307408 11.00000 0.02162 0.01872 =
0.01873 0.00163 0.00233 0.00130
C00K 1 0.739972 0.637756 0.318881 11.00000 0.02143 0.01600 =
0.02108 -0.00108 0.00232 0.00024
C00L 1 0.955771 0.375381 0.422897 11.00000 0.03447 0.02097 =
0.02456 -0.00034 -0.00197 -0.00304
C00M 1 0.379181 0.670616 0.313818 11.00000 0.02058 0.02212 =
0.02938 -0.00921 0.00285 -0.00469
C00N 1 0.594132 0.205537 0.471928 11.00000 0.02227 0.02390 =
0.01773 0.00169 -0.00001 -0.00117
C00O 1 0.804475 0.797775 0.302931 11.00000 0.02672 0.01579 =
0.02248 -0.00113 0.00567 0.00006
PART 2
N0 3 0.501206 0.268020 0.476801 10.50000 0.04411 0.05233 =
0.02456 0.01602 0.01208 -0.00119
PART 0
C00Q 1 0.585797 0.012228 0.308685 11.00000 0.02545 0.01816 =
0.02546 0.00206 0.00160 0.00075
C00R 1 0.513483 0.615073 0.028491 11.00000 0.03581 0.02437 =
0.02374 0.00126 -0.00150 -0.00419
C00S 1 0.818287 0.630438 0.372310 11.00000 0.03001 0.02029 =
0.02442 0.00272 -0.00313 -0.00191
C00T 1 0.389629 0.554733 0.128553 11.00000 0.02549 0.02824 =
0.02825 0.00192 -0.00142 -0.00631
C00U 1 0.423121 0.160713 0.276400 11.00000 0.02502 0.02722 =
0.03009 -0.00381 -0.00467 0.00650
C00V 1 0.890877 0.711431 0.389931 11.00000 0.03264 0.02636 =
0.02651 0.00034 -0.00570 -0.00451
C00W 1 0.471748 -0.013155 0.279773 11.00000 0.02924 0.02267 =
0.03081 -0.00420 0.00091 -0.00314
C00X 1 1.151976 0.331766 0.350384 11.00000 0.02585 0.02587 =
0.04381 -0.00292 -0.00106 -0.00265
C00Y 1 0.384407 0.601177 0.022531 11.00000 0.03703 0.03252 =
0.02899 0.00407 -0.01027 -0.00501
C00Z 1 0.376218 0.608146 0.364944 11.00000 0.04165 0.02992 =
0.03128 -0.00643 0.01177 -0.00826
C010 1 0.884308 0.797820 0.354551 11.00000 0.02908 0.02057 =
0.02681 -0.00357 0.00182 -0.00542
C011 1 1.077443 0.402637 0.441541 11.00000 0.04077 0.02301 =
0.03163 -0.00199 -0.00975 -0.00405
C012 1 0.389874 0.063901 0.262388 11.00000 0.02554 0.03330 =
0.03741 -0.00907 -0.00658 0.00054
C013 1 0.321903 0.569574 0.073710 11.00000 0.02744 0.03884 =
0.03665 0.00319 -0.00760 -0.00797
C014 1 1.178120 0.381036 0.404875 11.00000 0.03004 0.02605 =
0.04597 -0.00141 -0.01008 -0.00486
C015 1 0.419846 0.164552 0.556527 11.00000 0.02753 0.06609 =
0.03249 0.01887 0.00753 0.00112
C016 1 0.406929 0.247393 0.519736 11.00000 0.03546 0.06259 =
0.03569 0.01411 0.00925 0.01469
C017 1 0.521064 0.102426 0.547535 11.00000 0.03540 0.05107 =
0.03383 0.01933 0.00580 0.00099
C018 1 0.300752 0.635928 0.412406 11.00000 0.05184 0.04823 =
0.03653 -0.01638 0.01902 -0.02111
C019 1 0.242087 0.779603 0.355867 11.00000 0.02963 0.04689 =
0.05993 -0.02936 0.00543 0.00431
C01A 1 0.231912 0.722631 0.407792 11.00000 0.03765 0.06152 =
0.05002 -0.03283 0.01916 -0.01289
AFIX 6
O1 4 0.600506 0.520452 0.499040 10.50000 0.29561 0.06965 =
0.12221 -0.03648 -0.08344 0.07073
H1A 2 0.563099 0.566560 0.478866 10.50000 -1.50000
H1B 2 0.617512 0.473129 0.475004 10.50000 -1.50000
AFIX 0
H00L 2 0.885772 0.389512 0.447858 11.00000 0.03480
H00O 2 0.797283 0.854361 0.276614 11.00000 0.02355
H00R 2 0.562727 0.634810 -0.007774 11.00000 0.03878
H00T 2 0.349732 0.534420 0.164526 11.00000 0.03789
H00V 2 0.947177 0.706829 0.426436 11.00000 0.04002
H00Y 2 0.343432 0.611180 -0.014991 11.00000 0.04816
H00S 2 0.817948 0.568961 0.395609 11.00000 0.02816
H008 2 0.746282 0.179091 0.427628 11.00000 0.03179
H011 2 1.088263 0.438188 0.481175 11.00000 0.04095
H010 2 0.934819 0.857450 0.365251 11.00000 0.03666
H00X 2 1.220701 0.314396 0.320920 11.00000 0.04294
H00A 2 0.819480 0.267941 0.307044 11.00000 0.03552
H00D 2 0.674956 0.583945 0.181627 11.00000 0.03223
H013 2 0.229256 0.559064 0.072512 11.00000 0.04587
H00Q 2 0.645913 -0.038063 0.319934 11.00000 0.03341
H019 2 0.196481 0.837190 0.350086 11.00000 0.05845
H015 2 0.362031 0.148729 0.587722 11.00000 0.05822
H00Z 2 0.428440 0.546995 0.367022 11.00000 0.04609
H018 2 0.296413 0.595351 0.448237 11.00000 0.06200
H00B 2 0.668679 0.509493 0.326877 11.00000 0.03671
H00W 2 0.449333 -0.081538 0.272472 11.00000 0.03220
H00U 2 0.369354 0.215992 0.266153 11.00000 0.03901
H016 2 0.340616 0.292040 0.524573 11.00000 0.05631
H009 2 0.459676 0.694676 0.239115 11.00000 0.03850
H012 2 0.307381 0.049551 0.242106 11.00000 0.04120
H01A 2 0.176417 0.742217 0.439305 11.00000 0.06100
H017 2 0.531585 0.040834 0.571915 11.00000 0.05211
H00C 2 0.534729 0.323692 0.306603 11.00000 0.03747
PART 1
N0AA 3 0.599213 0.126837 0.504939 10.50000 0.01379 0.02758 =
0.02813 0.00616 0.00065 0.01119
C1 1 0.488221 0.268839 0.477573 10.50000 0.02232 0.03053 =
0.03783 0.00558 0.00432 0.01870
PART 0
H014 2 1.261443 0.397463 0.417266 11.00000 0.04881
H1 2 0.476907 0.324369 0.447600 11.00000 0.09131
H0 2 0.681689 0.070680 0.490753 11.00000 0.17927
HKLF 4
REM ms2k_c1_a.res in P2(1)/n
REM R1 = 0.0354 for 7346 Fo > 4sig(Fo) and 0.0359 for all 7572 data
REM 570 parameters refined using 2 restraints
END
WGHT 0.0551 1.1480
REM Highest difference peak 0.292, deepest hole -0.465, 1-sigma level 0.069
Q1 1 0.4204 0.2134 0.5458 11.00000 0.05 0.29
Q2 1 0.4874 0.6020 0.2597 11.00000 0.05 0.28
Q3 1 0.5717 0.5612 0.2154 11.00000 0.05 0.26
Q4 1 0.4360 0.0274 0.2692 11.00000 0.05 0.26
Q5 1 0.4722 0.1377 0.5532 11.00000 0.05 0.26
Q6 1 0.4043 0.1064 0.2799 11.00000 0.05 0.26
Q7 1 0.9464 0.3506 0.3952 11.00000 0.05 0.25
Q8 1 0.2582 0.6788 0.4022 11.00000 0.05 0.25
Q9 1 0.7669 0.3099 0.3585 11.00000 0.05 0.25
Q10 1 0.1949 0.7441 0.3807 11.00000 0.05 0.25
Q11 1 0.4147 0.6577 0.2905 11.00000 0.05 0.24
Q12 1 0.3319 0.6224 0.3875 11.00000 0.05 0.24
Q13 1 0.5852 0.1400 0.3164 11.00000 0.05 0.23
Q14 1 1.0180 0.3836 0.4378 11.00000 0.05 0.23
Q15 1 0.7340 0.6829 0.3001 11.00000 0.05 0.23
Q16 1 0.4550 0.5597 0.1300 11.00000 0.05 0.23
Q17 1 0.3612 0.1881 0.6043 11.00000 0.05 0.22
Q18 1 0.9929 0.3048 0.3516 11.00000 0.05 0.22
Q19 1 0.3741 0.6407 0.3447 11.00000 0.05 0.22
Q20 1 0.3237 0.2095 0.6221 11.00000 0.05 0.22
REM The information below was added by Olex2.
REM
REM R1 = 0.0354 for 7346 Fo > 4sig(Fo) and 0.0359 for all 45555 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.29, deepest hole -0.47
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0359
REM R1_gt = 0.0354
REM wR_ref = 0.0947
REM GOOF = 1.043
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 45555
REM Reflections_gt = 7346
REM Parameters = n/a
REM Hole = -0.47
REM Peak = 0.29
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_mb1k_c3__twin1
_database_code_depnum_ccdc_archive 'CCDC 1956237'
loop_
_audit_author_name
_audit_author_address
'Dan G Dumitrescu'
;Sincrotrone Elettra Trieste
Italy
;
_audit_update_record
;
2019-09-26 deposited with the CCDC. 2021-02-01 downloaded from the CCDC.
;
_audit_creation_date 2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C6 H6 Cu2 O12), C2 H8 N'
_chemical_formula_sum 'C5 H11 Cu N O6'
_chemical_formula_weight 244.69
_chemical_melting_point ?
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'
Cu Cu 0.3450 1.2548 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'I 1 2/a 1'
_space_group_name_Hall '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
_cell_length_a 11.5393(16)
_cell_length_b 8.6391(6)
_cell_length_c 8.8358(9)
_cell_angle_alpha 90
_cell_angle_beta 95.746(11)
_cell_angle_gamma 90
_cell_volume 876.41(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1136
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 31.1900
_cell_measurement_theta_min 2.7160
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.394
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.15306
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour light_blue
_exptl_crystal_density_diffrn 1.854
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 500
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0466
_diffrn_reflns_av_unetI/netI 0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 3048
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full 24.835
_diffrn_reflns_theta_max 31.758
_diffrn_reflns_theta_min 2.906
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 0.00 180.00 0.50 0.13 -- 0.00 0.00 0.00 360
;
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method 'rotating crystal'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.700
_diffrn_source SCW
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 951
_reflns_number_total 1239
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.371
_refine_diff_density_min -1.028
_refine_diff_density_rms 0.246
_refine_ls_extinction_coef 0.005(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.171
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 64
_refine_ls_number_reflns 1239
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0931
_refine_ls_R_factor_gt 0.0734
_refine_ls_restrained_S_all 1.171
_refine_ls_shift/su_max 0.033
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1996P)^2^+0.0925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2243
_refine_ls_wR_factor_ref 0.2824
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
N005(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
C006(H006), C008(H008)
3.c Idealised Me refined as rotating group:
C007(H00C,H00D,H00E)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
Cu01 Cu 0.500000 0.500000 0.000000 0.0356(5) Uani 1 2 d S T P . .
O002 O 0.3463(3) 0.3938(3) 0.0074(4) 0.0392(8) Uani 1 1 d . . . . .
O003 O 0.5717(3) 0.2320(3) 0.3797(4) 0.0394(8) Uani 1 1 d . . . . .
O004 O 0.5600(3) 0.4135(4) 0.2020(4) 0.0405(8) Uani 1 1 d . . . . .
N005 N 0.750000 0.4331(6) 0.500000 0.0400(13) Uani 1 2 d S T P . .
H00A H 0.696278 0.372463 0.451104 0.048 Uiso 0.5 1 calc R . . . .
H00B H 0.803723 0.372463 0.548896 0.048 Uiso 0.5 1 calc R . . . .
C006 C 0.5279(4) 0.2871(5) 0.2588(5) 0.0387(10) Uani 1 1 d . . . . .
H006 H 0.467358 0.232755 0.205441 0.046 Uiso 1 1 calc R . . . .
C007 C 0.6955(5) 0.5271(6) 0.6110(7) 0.0382(11) Uani 1 1 d . . . . .
H00C H 0.637721 0.593328 0.558880 0.057 Uiso 1 1 calc GR . . . .
H00D H 0.753704 0.589199 0.667583 0.057 Uiso 1 1 calc GR . . . .
H00E H 0.659195 0.460586 0.679398 0.057 Uiso 1 1 calc GR . . . .
C008 C 0.250000 0.4625(8) 0.000000 0.0388(14) Uani 1 2 d S T P . .
H008 H 0.250001 0.570154 -0.000001 0.047 Uiso 1 2 calc RS T P . .
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
Cu01 0.0692(8) 0.0110(6) 0.0258(6) 0.00282(19) 0.0008(4) -0.0031(2)
O002 0.078(2) 0.0107(14) 0.0293(15) -0.0003(10) 0.0055(14) -0.0010(12)
O003 0.069(2) 0.0147(13) 0.0343(15) -0.0015(12) 0.0022(13) 0.0036(12)
O004 0.068(2) 0.0187(14) 0.0339(16) -0.0013(12) 0.0029(14) -0.0038(13)
N005 0.072(4) 0.012(2) 0.033(3) 0.000 -0.009(2) 0.000
C006 0.064(3) 0.0137(17) 0.037(2) -0.0047(15) -0.0010(19) -0.0012(16)
C007 0.064(3) 0.0227(17) 0.030(2) 0.0021(19) 0.0181(19) -0.0012(19)
C008 0.076(4) 0.011(2) 0.028(3) 0.000 -0.001(2) 0.000
_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
Cu01 O002 2.004(4) 5_665 ?
Cu01 O002 2.004(4) . ?
Cu01 O004 1.994(3) 5_665 ?
Cu01 O004 1.994(3) . ?
O002 C008 1.256(5) . ?
O003 C006 1.231(6) . ?
O004 C006 1.272(5) . ?
N005 H00A 0.8900 . ?
N005 H00B 0.8900 . ?
N005 C007 1.463(6) . ?
N005 C007 1.463(6) 2_656 ?
C006 H006 0.9300 . ?
C007 H00C 0.9600 . ?
C007 H00D 0.9600 . ?
C007 H00E 0.9600 . ?
C008 H008 0.9300 . ?
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
O002 Cu01 O002 180.0 5_665 . ?
O004 Cu01 O002 91.62(13) 5_665 5_665 ?
O004 Cu01 O002 91.62(13) . . ?
O004 Cu01 O002 88.38(13) . 5_665 ?
O004 Cu01 O002 88.38(13) 5_665 . ?
O004 Cu01 O004 180.0 5_665 . ?
C008 O002 Cu01 124.3(3) . . ?
C006 O004 Cu01 125.9(3) . . ?
H00A N005 H00B 107.8 . . ?
C007 N005 H00A 109.1 . . ?
C007 N005 H00A 109.1 2_656 . ?
C007 N005 H00B 109.1 . . ?
C007 N005 H00B 109.1 2_656 . ?
C007 N005 C007 112.6(5) . 2_656 ?
O003 C006 O004 124.3(4) . . ?
O003 C006 H006 117.9 . . ?
O004 C006 H006 117.9 . . ?
N005 C007 H00C 109.5 . . ?
N005 C007 H00D 109.5 . . ?
N005 C007 H00E 109.5 . . ?
H00C C007 H00D 109.5 . . ?
H00C C007 H00E 109.5 . . ?
H00D C007 H00E 109.5 . . ?
O002 C008 O002 123.6(6) 2 . ?
O002 C008 H008 118.2 2 . ?
O002 C008 H008 118.2 . . ?
_iucr_refine_instructions_details
;
TITL mb1k_c3__twin1_a.res in I2/a
mb1k_c3__twin1.res
created by SHELXL-2018/3 at 15:55:45 on 24-Jul-2019
REM Old TITL MB1K_c3__twin1 in I2/a
REM SHELXT solution in I2/a
REM R1 0.467, Rweak 0.491, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: C5 N O6 Cu
CELL 0.7 11.5393 8.6391 8.8358 90 95.746 90
ZERR 4 0.0016 0.0006 0.0009 0 0.011 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
DISP C 0.0033 0.0016 11.1819
DISP Cu 0.345 1.2548 4976.3916
DISP H -0 0 0.6234
DISP N 0.0063 0.0031 18.9823
DISP O 0.0112 0.0059 31.3712
UNIT 20 44 4 4 24
L.S. 4
PLAN 20
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.199600 0.092500
EXTI 0.000000
FVAR 0.62904
CU01 3 0.500000 0.500000 0.000000 10.50000 0.06920 0.01101 =
0.02583 0.00282 0.00083 -0.00308
O002 5 0.346296 0.393807 0.007444 11.00000 0.07759 0.01068 =
0.02929 -0.00029 0.00552 -0.00102
O003 5 0.571741 0.232033 0.379736 11.00000 0.06856 0.01466 =
0.03431 -0.00147 0.00219 0.00357
O004 5 0.560003 0.413502 0.202019 11.00000 0.06845 0.01867 =
0.03392 -0.00132 0.00288 -0.00379
N005 4 0.750000 0.433140 0.500000 10.50000 0.07222 0.01189 =
0.03283 0.00000 -0.00949 0.00000
AFIX 23
H00A 2 0.696278 0.372463 0.451104 10.50000 -1.20000
H00B 2 0.803723 0.372463 0.548896 10.50000 -1.20000
AFIX 0
C006 1 0.527904 0.287116 0.258786 11.00000 0.06392 0.01371 =
0.03736 -0.00470 -0.00103 -0.00123
AFIX 43
H006 2 0.467358 0.232755 0.205441 11.00000 -1.20000
AFIX 0
C007 1 0.695466 0.527147 0.611011 11.00000 0.06439 0.02266 =
0.03030 0.00208 0.01806 -0.00120
AFIX 137
H00C 2 0.637721 0.593328 0.558880 11.00000 -1.50000
H00D 2 0.753704 0.589199 0.667583 11.00000 -1.50000
H00E 2 0.659195 0.460586 0.679398 11.00000 -1.50000
AFIX 0
C008 1 0.250000 0.462504 0.000000 10.50000 0.07604 0.01103 =
0.02818 0.00000 -0.00055 0.00000
AFIX 43
H008 2 0.250001 0.570154 -0.000001 10.50000 -1.20000
AFIX 0
HKLF 4
REM mb1k_c3__twin1_a.res in I2/a
REM wR2 = 0.2824, GooF = S = 1.171, Restrained GooF = 1.171 for all data
REM R1 = 0.0734 for 951 Fo > 4sig(Fo) and 0.0931 for all 1239 data
REM 64 parameters refined using 0 restraints
END
WGHT 0.1993 0.1129
REM Highest difference peak 1.371, deepest hole -1.028, 1-sigma level 0.246
Q1 1 0.5669 0.5631 -0.0204 11.00000 0.05 1.37
Q2 1 0.4363 0.5616 0.0211 11.00000 0.05 1.34
Q3 1 0.6394 0.2914 0.3510 11.00000 0.05 0.80
Q4 1 0.7636 0.5041 0.5830 11.00000 0.05 0.77
Q5 1 0.6119 0.3674 0.1808 11.00000 0.05 0.77
Q6 1 0.6609 0.2038 0.3762 11.00000 0.05 0.74
Q7 1 0.5241 0.2706 0.4261 11.00000 0.05 0.73
Q8 1 0.5758 0.5039 0.8092 11.00000 0.05 0.72
Q9 1 0.5489 0.4558 0.0961 11.00000 0.05 0.69
Q10 1 0.6484 0.4943 0.1696 11.00000 0.05 0.69
Q11 1 0.5834 0.5055 0.1080 11.00000 0.05 0.68
Q12 1 0.6091 0.2008 0.3164 11.00000 0.05 0.67
Q13 1 0.6045 0.4846 0.3184 11.00000 0.05 0.66
Q14 1 0.6475 0.5380 0.6391 11.00000 0.05 0.63
Q15 1 0.8497 0.4559 0.6569 11.00000 0.05 0.62
Q16 1 0.5360 0.5680 0.0886 11.00000 0.05 0.61
Q17 1 0.5395 0.5012 0.4608 11.00000 0.05 0.60
Q18 1 0.4345 0.2253 0.2033 11.00000 0.05 0.60
Q19 1 0.4897 0.4728 0.2585 11.00000 0.05 0.58
Q20 1 0.3718 0.2003 0.1578 11.00000 0.05 0.58
REM The information below was added by Olex2.
REM
REM R1 = 0.0734 for 951 Fo > 4sig(Fo) and 0.0931 for all 3147 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.37, deepest hole -1.03
REM Mean Shift 0.001, Max Shift -0.033.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0931
REM R1_gt = 0.0734
REM wR_ref = 0.2824
REM GOOF = 1.171
REM Shift_max = -0.033
REM Shift_mean = 0.001
REM Reflections_all = 3147
REM Reflections_gt = 951
REM Parameters = n/a
REM Hole = -1.03
REM Peak = 1.37
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#######################################################################
#
# 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_ms2kstar_c2
_database_code_depnum_ccdc_archive 'CCDC 1960317'
loop_
_audit_author_name
_audit_author_address
'Dan G. Dumitrescu '
;XRD beamline, Elettra Sincrotrone, Trieste
Italy
;
_audit_update_record
;
2019-10-19 deposited with the CCDC. 2021-02-01 downloaded from the CCDC.
;
_audit_creation_date 2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C15 H15 N6 O P '
_chemical_formula_sum 'C15 H15 N6 O P '
_chemical_formula_weight 326.3
_chemical_melting_point ?
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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1453 0.1556 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3441 0.7121 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_H-M_alt 'R -3'
_space_group_name_Hall '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 10.0040(14)
_cell_length_b 10.0040(14)
_cell_length_c 28.420(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 2463.2(8)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 9808
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.644
_cell_measurement_theta_min 2.117
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.172
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.32
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1422
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0401
_diffrn_reflns_av_unetI/netI 0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_number 11986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 24.835
_diffrn_reflns_theta_max 27.644
_diffrn_reflns_theta_min 2.117
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Arinax MD2S/Pilatus 6M'
_diffrn_measurement_method 'rotating crystal'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.700
_diffrn_source SCW
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1325
_reflns_number_total 1340
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.502
_refine_diff_density_min -0.447
_refine_diff_density_rms 0.071
_refine_ls_extinction_coef 0.0177(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 91
_refine_ls_number_reflns 1340
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0375
_refine_ls_R_factor_gt 0.0373
_refine_ls_restrained_S_all 1.085
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+3.4472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1088
_refine_ls_wR_factor_ref 0.1090
_refine_special_details ?
_olex2_refinement_description
;
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
P001 P 1.000000 1.000000 0.74226(2) 0.0096(2) Uani 1 3 d S T P . .
O002 O 1.000000 1.000000 0.79428(5) 0.0128(3) Uani 1 3 d S T P . .
N003 N 0.89576(11) 0.82560(11) 0.71918(3) 0.0118(2) Uani 1 1 d . . . . .
N004 N 0.67581(12) 0.59076(12) 0.70494(3) 0.0163(3) Uani 1 1 d . . . . .
C005 C 0.74775(13) 0.71153(13) 0.73412(4) 0.0127(3) Uani 1 1 d . . . . .
C006 C 0.68159(14) 0.72287(14) 0.77625(4) 0.0203(3) Uani 1 1 d . . . . .
C007 C 0.53593(17) 0.60405(18) 0.78831(5) 0.0310(4) Uani 1 1 d . . . . .
C008 C 0.53483(16) 0.47676(16) 0.71772(5) 0.0255(3) Uani 1 1 d . . . . .
C009 C 0.46077(18) 0.47761(18) 0.75851(6) 0.0341(4) Uani 1 1 d . . . . .
H006 H 0.742(2) 0.814(2) 0.7950(6) 0.030(5) Uiso 1 1 d . . . . .
H009 H 0.356(3) 0.389(3) 0.7650(8) 0.044(6) Uiso 1 1 d . . . . .
H007 H 0.479(3) 0.608(2) 0.8167(7) 0.040(5) Uiso 1 1 d . . . . .
H003 H 0.926(2) 0.804(2) 0.6948(8) 0.035(5) Uiso 1 1 d . . . . .
H008 H 0.488(2) 0.392(2) 0.6965(7) 0.030(5) Uiso 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
P001 0.0099(2) 0.0099(2) 0.0091(3) 0.000 0.000 0.00496(11)
O002 0.0148(4) 0.0148(4) 0.0089(6) 0.000 0.000 0.0074(2)
N003 0.0117(5) 0.0112(4) 0.0111(5) -0.0006(3) 0.0021(3) 0.0047(4)
N004 0.0151(5) 0.0137(5) 0.0164(5) -0.0024(4) 0.0025(4) 0.0045(4)
C005 0.0118(5) 0.0116(5) 0.0143(5) -0.0001(4) 0.0012(4) 0.0055(4)
C006 0.0168(6) 0.0174(6) 0.0202(6) -0.0061(4) 0.0052(4) 0.0035(5)
C007 0.0224(7) 0.0269(7) 0.0280(7) -0.0104(6) 0.0127(5) 0.0007(6)
C008 0.0199(6) 0.0187(6) 0.0254(7) -0.0082(5) 0.0057(5) 0.0002(5)
C009 0.0208(7) 0.0251(7) 0.0349(8) -0.0111(6) 0.0133(6) -0.0046(6)
_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
P001 O002 1.4784(14) . ?
P001 N003 1.6560(10) 2_765 ?
P001 N003 1.6560(10) . ?
P001 N003 1.6560(10) 3_675 ?
N003 C005 1.4090(14) . ?
N003 H003 0.82(2) . ?
N004 C005 1.3401(15) . ?
N004 C008 1.3465(16) . ?
C005 C006 1.4000(16) . ?
C006 C007 1.3862(18) . ?
C006 H006 0.97(2) . ?
C007 C009 1.3897(19) . ?
C007 H007 1.00(2) . ?
C008 C009 1.3783(19) . ?
C008 H008 0.95(2) . ?
C009 H009 0.99(2) . ?
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
O002 P001 N003 113.34(4) . . ?
O002 P001 N003 113.34(4) . 3_675 ?
O002 P001 N003 113.34(4) . 2_765 ?
N003 P001 N003 105.34(4) . 3_675 ?
N003 P001 N003 105.34(4) . 2_765 ?
N003 P001 N003 105.34(4) 2_765 3_675 ?
P001 N003 H003 119.0(15) . . ?
C005 N003 P001 125.95(8) . . ?
C005 N003 H003 114.6(15) . . ?
C005 N004 C008 117.36(10) . . ?
N004 C005 N003 114.64(10) . . ?
N004 C005 C006 122.67(11) . . ?
C006 C005 N003 122.69(10) . . ?
C005 C006 H006 117.0(12) . . ?
C007 C006 C005 118.60(11) . . ?
C007 C006 H006 124.4(12) . . ?
C006 C007 C009 119.23(12) . . ?
C006 C007 H007 122.7(13) . . ?
C009 C007 H007 118.0(13) . . ?
N004 C008 C009 124.07(12) . . ?
N004 C008 H008 115.0(12) . . ?
C009 C008 H008 121.0(12) . . ?
C007 C009 H009 123.3(13) . . ?
C008 C009 C007 118.06(13) . . ?
C008 C009 H009 118.6(13) . . ?
_iucr_refine_instructions_details
;
TITL ms2kstar_c2_a.res in R-3
ms2kstar_c2.res
created by SHELXL-2018/1 at 18:40:37 on 26-Jun-2019
REM Old TITL MS2Kstar_c2 in R-3
REM SHELXT solution in R-3
REM R1 0.110, Rweak 0.008, Alpha 0.031, Orientation as input
REM Formula found by SHELXT: C15 N6 O P
CELL 0.7 10.004 10.004 28.42 90 90 120
ZERR 18 0.0014 0.0014 0.0057 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H N O P Cl Mn
DISP C 0.0033 0.0016 11.1819
DISP Cl 0.1453 0.1556 651.6741
DISP H -0 0 0.6234
DISP Mn 0.3441 0.7121 2905.5343
DISP N 0.0063 0.0031 18.9823
DISP O 0.0112 0.0059 31.3712
DISP P 0.1018 0.0938 394.0833
UNIT 18 18 18 18 18 18 18
L.S. 10
PLAN 20
BOND $H
LIST 6
fmap 2
ACTA
REM
REM
REM
WGHT 0.066100 3.447200
EXTI 0.017695
FVAR 0.44424
P001 5 1.000000 1.000000 0.742259 10.33333 0.00991 0.00991 =
0.00909 0.00000 0.00000 0.00496
O002 4 1.000000 1.000000 0.794278 10.33333 0.01476 0.01476 =
0.00892 0.00000 0.00000 0.00738
N003 3 0.895761 0.825604 0.719176 11.00000 0.01166 0.01122 =
0.01107 -0.00064 0.00210 0.00471
N004 3 0.675812 0.590761 0.704939 11.00000 0.01513 0.01368 =
0.01636 -0.00237 0.00248 0.00447
C005 1 0.747754 0.711526 0.734120 11.00000 0.01183 0.01158 =
0.01426 -0.00010 0.00116 0.00555
C006 1 0.681590 0.722872 0.776255 11.00000 0.01675 0.01739 =
0.02016 -0.00606 0.00516 0.00353
C007 1 0.535929 0.604047 0.788309 11.00000 0.02240 0.02694 =
0.02801 -0.01043 0.01274 0.00069
C008 1 0.534832 0.476758 0.717715 11.00000 0.01994 0.01866 =
0.02539 -0.00821 0.00568 0.00023
C009 1 0.460772 0.477612 0.758512 11.00000 0.02079 0.02508 =
0.03488 -0.01109 0.01327 -0.00460
H006 2 0.741647 0.814196 0.795034 11.00000 0.02958
H009 2 0.356402 0.388870 0.765000 11.00000 0.04449
H007 2 0.479404 0.608007 0.816715 11.00000 0.03969
H003 2 0.926000 0.804404 0.694839 11.00000 0.03468
H008 2 0.488309 0.391841 0.696451 11.00000 0.03025
HKLF 4
REM ms2kstar_c2_a.res in R-3
REM R1 = 0.0373 for 1325 Fo > 4sig(Fo) and 0.0375 for all 1340 data
REM 91 parameters refined using 0 restraints
END
WGHT 0.0661 3.4403
REM Highest difference peak 0.502, deepest hole -0.447, 1-sigma level 0.071
Q1 1 0.3631 0.6338 0.6740 11.00000 0.05 0.50
Q2 1 0.9415 0.8986 0.7321 11.00000 0.05 0.38
Q3 1 0.6109 0.6673 0.7801 11.00000 0.05 0.37
Q4 1 0.7180 0.7151 0.7573 11.00000 0.05 0.35
Q5 1 0.8200 0.7757 0.7280 11.00000 0.05 0.34
Q6 1 0.4938 0.5425 0.7718 11.00000 0.05 0.34
Q7 1 0.7139 0.6479 0.7203 11.00000 0.05 0.29
Q8 1 0.6104 0.5429 0.7119 11.00000 0.05 0.27
Q9 1 0.4973 0.4894 0.7363 11.00000 0.05 0.26
Q10 1 0.6667 0.3333 0.8333 10.16667 0.05 0.22
Q11 1 0.6667 0.3333 0.8036 10.33333 0.05 0.21
Q12 1 0.3337 0.4310 0.7582 11.00000 0.05 0.16
Q13 1 0.7196 0.5539 0.7063 11.00000 0.05 0.16
Q14 1 0.4544 0.4140 0.6875 11.00000 0.05 0.16
Q15 1 0.9532 1.0049 0.7772 11.00000 0.05 0.15
Q16 1 0.7212 0.5821 0.6846 11.00000 0.05 0.13
Q17 1 0.4070 0.3760 0.7737 11.00000 0.05 0.12
Q18 1 0.2466 0.2523 0.7484 11.00000 0.05 0.12
Q19 1 0.4189 0.6934 0.7283 11.00000 0.05 0.11
Q20 1 0.2711 0.4268 0.7475 11.00000 0.05 0.11
REM The information below was added by Olex2.
REM
REM R1 = 0.0373 for 1325 Fo > 4sig(Fo) and 0.0375 for all 11986 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.50, deepest hole -0.45
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0375
REM R1_gt = 0.0373
REM wR_ref = 0.1090
REM GOOF = 1.085
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 11986
REM Reflections_gt = 1325
REM Parameters = n/a
REM Hole = -0.45
REM Peak = 0.50
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_ms3k_c2
_database_code_depnum_ccdc_archive 'CCDC 1956238'
loop_
_audit_author_name
_audit_author_address
'Dan G Dumitrescu'
;Sincrotrone Elettra Trieste
Italy
;
_audit_update_record
;
2019-09-26 deposited with the CCDC. 2021-02-01 downloaded from the CCDC.
;
_audit_creation_date 2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C30 H32 Co N12 O2 P2, 3.053(Cl)'
_chemical_formula_sum 'C30 H32 Cl3.05 Co N12 O2 P2'
_chemical_formula_weight 821.77
_chemical_melting_point ?
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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1453 0.1556 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3554 0.9393 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 8.5130(17)
_cell_length_b 15.816(3)
_cell_length_c 26.981(5)
_cell_angle_alpha 90
_cell_angle_beta 93.06(3)
_cell_angle_gamma 90
_cell_volume 3627.6(13)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 58514
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.666
_cell_measurement_theta_min 1.470
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.793
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.505
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1683.6
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.04
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0228
_diffrn_reflns_av_unetI/netI 0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 51573
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full 24.835
_diffrn_reflns_theta_max 27.666
_diffrn_reflns_theta_min 1.470
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type 'Arinax MD2S/Pilatus 6M'
_diffrn_measurement_method 'rotating crystal'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.700
_diffrn_source SCW
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7105
_reflns_number_total 8709
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.936
_refine_diff_density_min -0.670
_refine_diff_density_rms 0.091
_refine_ls_extinction_coef 0.0096(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 528
_refine_ls_number_reflns 8709
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0576
_refine_ls_R_factor_gt 0.0492
_refine_ls_restrained_S_all 1.040
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+3.1761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1503
_refine_ls_wR_factor_ref 0.1598
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
2. Others
1*[Sof(Cl01)]+1*[Sof(Cl3)]+1*[Sof(Cl1)]+1*[Sof(Cl06)]+1*[Sof(Cl0A)]+1*
[Sof(Cl2)]+1*[Sof(Cl4)]+1*[Sof(Cl1A)]+1*[Sof(Cl05)]+1*[Sof(Cl2A)]=3 with esd
of 0.01
1*[Sof(Cl01)]+1*[Sof(Cl3)]+1*[Sof(Cl1)]+1*[Sof(Cl06)]+1*[Sof(Cl0A)]+1*
[Sof(Cl2)]+1*[Sof(Cl4)]+1*[Sof(Cl1A)]+1*[Sof(Cl05)]+1*[Sof(Cl2A)]=3 with esd
of 0.01
3.a Aromatic/amide H refined with riding coordinates:
N00D(H00D), N00E(H00E), N00F(H00F), N00G(H00G), N00H(H00H), N00I(H00I),
N00J(H00J), N00K(H00K), C00L(H00L), C00N(H00N), C00Q(H00Q), C00S(H00S),
C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y),
C00Z(H00Z), C010(H010), C012(H012), C013(H013), C014(H014), C015(H015),
C016(H016), C017(H017), C01A(H01A), C01D(H01D), C01E(H01E), C01F(H01F),
C01G(H01G), C01H(H01H)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
Co01 Co 0.500000 0.000000 0.500000 0.02727(13) Uani 1 2 d S T P . .
Co02 Co 0.000000 0.500000 0.500000 0.02897(13) Uani 1 2 d S T P . .
P003 P 0.10279(6) 0.45179(3) 0.39742(2) 0.03202(15) Uani 1 1 d . . . . .
P004 P 0.61494(6) 0.04898(3) 0.39919(2) 0.03102(15) Uani 1 1 d . . . . .
Cl05 Cl 0.60600(12) -0.22771(6) 0.21277(3) 0.0432(3) Uani 0.654(3) 1 d . . . .
.
Cl06 Cl 0.3789(2) 0.10907(10) 0.22544(8) 0.0413(9) Uani 0.461(11) 1 d . . . . .
O007 O 0.66080(17) 0.03993(9) 0.45334(6) 0.0324(3) Uani 1 1 d . . . . .
O008 O 0.15332(17) 0.45789(9) 0.45143(6) 0.0341(3) Uani 1 1 d . . . . .
N009 N 0.4477(2) -0.10707(10) 0.44907(7) 0.0312(4) Uani 1 1 d . . . . .
N00A N 0.3154(2) 0.07337(11) 0.45550(7) 0.0311(4) Uani 1 1 d . . . . .
N00B N -0.1910(2) 0.42953(11) 0.45769(7) 0.0326(4) Uani 1 1 d . . . . .
N00C N -0.0551(2) 0.60820(11) 0.45012(7) 0.0332(4) Uani 1 1 d . . . . .
N00D N 0.2192(2) 0.41649(12) 0.35892(8) 0.0385(4) Uani 1 1 d . . . . .
H00D H 0.193715 0.369970 0.344065 0.046 Uiso 1 1 calc R . . . .
N00E N 0.7383(2) 0.08329(12) 0.36252(7) 0.0376(4) Uani 1 1 d . . . . .
H00E H 0.720049 0.132035 0.349307 0.045 Uiso 1 1 calc R . . . .
N00F N 0.5522(2) -0.04443(11) 0.37794(8) 0.0361(4) Uani 1 1 d . . . . .
H00F H 0.571024 -0.053750 0.347418 0.043 Uiso 1 1 calc R . . . .
N00G N 0.4727(2) 0.12013(12) 0.39166(7) 0.0381(4) Uani 1 1 d . . . . .
H00G H 0.487683 0.160037 0.370776 0.046 Uiso 1 1 calc R . . . .
N00H N 0.0454(2) 0.54742(12) 0.37797(8) 0.0380(4) Uani 1 1 d . . . . .
H00H H 0.067172 0.558642 0.347913 0.046 Uiso 1 1 calc R . . . .
N00I N -0.0467(2) 0.38429(12) 0.39060(7) 0.0376(4) Uani 1 1 d . . . . .
H00I H -0.039124 0.346336 0.368026 0.045 Uiso 1 1 calc R . . . .
N00J N 0.4304(3) 0.41504(14) 0.31029(8) 0.0465(5) Uani 1 1 d . . . . .
H00J H 0.386912 0.371864 0.295847 0.056 Uiso 1 1 calc R . . . .
N00K N 0.9509(3) 0.08039(14) 0.31424(8) 0.0449(5) Uani 1 1 d . . . . .
H00K H 0.913771 0.126111 0.300937 0.054 Uiso 1 1 calc R . . . .
C00L C 0.4269(3) -0.17941(14) 0.37011(10) 0.0386(5) Uani 1 1 d . . . . .
H00L H 0.450781 -0.180729 0.336882 0.046 Uiso 1 1 calc R . . . .
C00M C 0.4747(2) -0.11024(13) 0.40062(9) 0.0324(4) Uani 1 1 d . . . . .
C00N C -0.0828(3) 0.68183(14) 0.37181(10) 0.0416(5) Uani 1 1 d . . . . .
H00N H -0.061495 0.683948 0.338381 0.050 Uiso 1 1 calc R . . . .
C00O C -0.0313(2) 0.61235(13) 0.40159(9) 0.0347(5) Uani 1 1 d . . . . .
C00P C 0.3326(3) 0.12224(13) 0.41533(8) 0.0335(4) Uani 1 1 d . . . . .
C00Q C 0.1729(2) 0.07435(14) 0.47579(9) 0.0373(5) Uani 1 1 d . . . . .
H00Q H 0.158496 0.039746 0.503037 0.045 Uiso 1 1 calc R . . . .
C00R C -0.1818(3) 0.38191(13) 0.41691(8) 0.0336(4) Uani 1 1 d . . . . .
C00S C -0.3306(2) 0.42855(14) 0.48031(10) 0.0378(5) Uani 1 1 d . . . . .
H00S H -0.339739 0.462475 0.508160 0.045 Uiso 1 1 calc R . . . .
C00T C 0.3445(3) -0.24469(14) 0.39029(10) 0.0431(5) Uani 1 1 d . . . . .
H00T H 0.309565 -0.290051 0.370719 0.052 Uiso 1 1 calc R . . . .
C00U C -0.1649(3) 0.74618(14) 0.39310(12) 0.0474(6) Uani 1 1 d . . . . .
H00U H -0.202323 0.791617 0.374041 0.057 Uiso 1 1 calc R . . . .
C00V C 0.3696(3) -0.17331(13) 0.46813(9) 0.0374(5) Uani 1 1 d . . . . .
H00V H 0.352069 -0.172687 0.501862 0.045 Uiso 1 1 calc R . . . .
C00W C -0.4444(3) 0.32901(14) 0.42361(10) 0.0430(6) Uani 1 1 d . . . . .
H00W H -0.527674 0.294675 0.412480 0.052 Uiso 1 1 calc R . . . .
C00X C -0.4589(3) 0.38056(15) 0.46456(10) 0.0434(5) Uani 1 1 d . . . . .
H00X H -0.552215 0.382763 0.480929 0.052 Uiso 1 1 calc R . . . .
C00Y C -0.3065(3) 0.32886(14) 0.39956(10) 0.0408(5) Uani 1 1 d . . . . .
H00Y H -0.295205 0.294231 0.372122 0.049 Uiso 1 1 calc R . . . .
C00Z C 0.0699(3) 0.17656(15) 0.41831(10) 0.0451(6) Uani 1 1 d . . . . .
H00Z H -0.010877 0.211931 0.406416 0.054 Uiso 1 1 calc R . . . .
C010 C 0.0475(3) 0.12396(15) 0.45825(11) 0.0448(6) Uani 1 1 d . . . . .
H010 H -0.048757 0.121892 0.472940 0.054 Uiso 1 1 calc R . . . .
Cl01 Cl 0.2429(3) 0.29365(18) 0.24897(10) 0.0757(9) Uani 0.361(3) 1 d . . . . .
C012 C 0.9344(3) -0.03109(17) 0.37115(10) 0.0453(6) Uani 1 1 d . . . . .
H012 H 0.884517 -0.058768 0.396339 0.054 Uiso 1 1 calc R . . . .
C013 C -0.1330(3) 0.67352(14) 0.47017(10) 0.0408(5) Uani 1 1 d . . . . .
H013 H -0.148433 0.672008 0.504024 0.049 Uiso 1 1 calc R . . . .
C014 C 0.4291(3) 0.52337(17) 0.36978(10) 0.0446(5) Uani 1 1 d . . . . .
H014 H 0.382315 0.551346 0.395487 0.054 Uiso 1 1 calc R . . . .
C015 C -0.1911(3) 0.74230(15) 0.44330(11) 0.0472(6) Uani 1 1 d . . . . .
H015 H -0.246253 0.784895 0.458560 0.057 Uiso 1 1 calc R . . . .
C016 C 0.3143(3) -0.24171(14) 0.44039(10) 0.0432(5) Uani 1 1 d . . . . .
H016 H 0.258263 -0.284734 0.454935 0.052 Uiso 1 1 calc R . . . .
C017 C 0.2116(3) 0.17648(14) 0.39621(10) 0.0418(5) Uani 1 1 d . . . . .
H017 H 0.227791 0.211371 0.369208 0.050 Uiso 1 1 calc R . . . .
C018 C 0.8683(3) 0.04320(15) 0.35027(9) 0.0384(5) Uani 1 1 d . . . . .
C019 C 0.3540(3) 0.45284(15) 0.34745(9) 0.0387(5) Uani 1 1 d . . . . .
C01A C 0.5706(3) 0.55140(19) 0.35403(11) 0.0524(6) Uani 1 1 d . . . . .
H01A H 0.618586 0.598358 0.369058 0.063 Uiso 1 1 calc R . . . .
Cl1 Cl 0.5279(4) 0.22256(19) 0.30463(11) 0.0749(11) Uani 0.331(4) 1 d . . . . .
Cl2 Cl 0.5818(5) -0.0526(3) 0.27223(11) 0.0966(15) Uani 0.398(5) 1 d . . . . .
C01D C 1.0884(3) 0.04977(19) 0.29797(10) 0.0495(6) Uani 1 1 d . . . . .
H01D H 1.139494 0.078710 0.273519 0.059 Uiso 1 1 calc R . . . .
C01E C 1.0720(3) -0.0629(2) 0.35456(11) 0.0529(6) Uani 1 1 d . . . . .
H01E H 1.113685 -0.112414 0.368454 0.063 Uiso 1 1 calc R . . . .
C01F C 0.5714(3) 0.4417(2) 0.29472(10) 0.0524(7) Uani 1 1 d . . . . .
H01F H 0.618455 0.412554 0.269492 0.063 Uiso 1 1 calc R . . . .
C01G C 0.6438(3) 0.5098(2) 0.31547(11) 0.0531(7) Uani 1 1 d . . . . .
H01G H 0.739383 0.528793 0.304538 0.064 Uiso 1 1 calc R . . . .
C01H C 1.1509(3) -0.0222(2) 0.31705(11) 0.0522(6) Uani 1 1 d . . . . .
H01H H 1.243654 -0.044159 0.305669 0.063 Uiso 1 1 calc R . . . .
Cl3 Cl 0.3992(5) 0.2277(2) 0.28709(11) 0.0451(13) Uani 0.180(3) 1 d . . . . .
Cl4 Cl 0.6227(6) -0.1106(4) 0.27502(17) 0.0594(19) Uani 0.172(5) 1 d . . . . .
Cl2A Cl 0.7495(12) -0.2937(7) 0.2510(4) 0.073(4) Uani 0.089(3) 1 d . . . . .
Cl1A Cl 0.4764(15) -0.2215(8) 0.1991(4) 0.080(5) Uani 0.087(4) 1 d . . . . .
Cl0A Cl 0.4253(17) 0.0692(15) 0.2336(3) 0.155(7) Uani 0.320(13) 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
Co01 0.0189(2) 0.0220(2) 0.0406(2) 0.00219(14) -0.00144(15) -0.00054(12)
Co02 0.0184(2) 0.0217(2) 0.0466(3) -0.00254(14) -0.00145(15) 0.00076(12)
P003 0.0265(3) 0.0229(3) 0.0467(3) 0.0007(2) 0.0027(2) 0.00038(18)
P004 0.0275(3) 0.0237(3) 0.0419(3) 0.0007(2) 0.0025(2) -0.00028(18)
Cl05 0.0514(7) 0.0333(5) 0.0455(5) -0.0024(3) 0.0077(4) 0.0002(4)
Cl06 0.0448(11) 0.0351(13) 0.0456(9) -0.0122(5) 0.0187(6) -0.0093(6)
O007 0.0229(7) 0.0299(7) 0.0444(8) 0.0032(6) 0.0000(6) -0.0046(5)
O008 0.0239(7) 0.0298(7) 0.0485(9) -0.0040(6) -0.0005(6) 0.0040(5)
N009 0.0232(8) 0.0212(8) 0.0485(10) 0.0012(7) -0.0038(7) 0.0015(6)
N00A 0.0235(8) 0.0241(8) 0.0451(10) -0.0024(7) -0.0050(7) 0.0017(6)
N00B 0.0228(8) 0.0237(8) 0.0506(10) 0.0021(7) -0.0047(7) -0.0015(6)
N00C 0.0220(8) 0.0212(8) 0.0558(11) -0.0007(7) -0.0041(7) -0.0008(6)
N00D 0.0363(10) 0.0288(9) 0.0510(11) -0.0021(8) 0.0081(8) 0.0009(7)
N00E 0.0376(10) 0.0286(9) 0.0471(10) 0.0030(8) 0.0080(8) -0.0024(7)
N00F 0.0343(10) 0.0291(9) 0.0453(10) -0.0054(7) 0.0067(8) -0.0043(7)
N00G 0.0393(10) 0.0316(9) 0.0435(10) 0.0062(8) 0.0035(8) 0.0095(8)
N00H 0.0330(10) 0.0284(9) 0.0531(11) 0.0079(8) 0.0081(8) 0.0041(7)
N00I 0.0394(10) 0.0295(9) 0.0438(10) -0.0030(8) 0.0016(8) -0.0081(8)
N00J 0.0495(12) 0.0465(12) 0.0444(11) 0.0036(9) 0.0112(9) 0.0079(9)
N00K 0.0486(12) 0.0422(11) 0.0448(11) -0.0022(9) 0.0101(9) -0.0055(9)
C00L 0.0327(11) 0.0286(10) 0.0540(13) -0.0068(9) -0.0016(9) 0.0038(8)
C00M 0.0211(9) 0.0233(9) 0.0526(12) -0.0022(8) -0.0013(8) 0.0027(7)
C00N 0.0331(11) 0.0292(11) 0.0621(15) 0.0088(10) -0.0014(10) -0.0024(9)
C00O 0.0205(9) 0.0227(9) 0.0606(14) 0.0040(9) -0.0004(8) -0.0023(7)
C00P 0.0325(11) 0.0236(9) 0.0432(11) -0.0039(8) -0.0072(8) 0.0036(8)
C00Q 0.0240(10) 0.0319(10) 0.0557(13) -0.0005(9) -0.0025(9) 0.0028(8)
C00R 0.0305(10) 0.0229(9) 0.0467(11) 0.0050(8) -0.0060(8) -0.0026(7)
C00S 0.0228(10) 0.0312(10) 0.0590(14) 0.0008(9) -0.0016(9) -0.0007(8)
C00T 0.0357(12) 0.0241(10) 0.0682(16) -0.0060(10) -0.0079(10) -0.0002(8)
C00U 0.0359(12) 0.0235(10) 0.0815(19) 0.0082(11) -0.0081(11) 0.0023(9)
C00V 0.0329(11) 0.0248(10) 0.0538(13) 0.0048(9) -0.0039(9) -0.0024(8)
C00W 0.0303(11) 0.0292(10) 0.0679(16) 0.0066(10) -0.0117(10) -0.0086(8)
C00X 0.0241(11) 0.0349(11) 0.0707(16) 0.0050(11) -0.0040(10) -0.0037(8)
C00Y 0.0391(12) 0.0276(10) 0.0543(13) 0.0031(9) -0.0100(10) -0.0070(9)
C00Z 0.0348(12) 0.0306(11) 0.0678(16) -0.0049(10) -0.0166(10) 0.0100(9)
C010 0.0263(11) 0.0354(12) 0.0720(17) -0.0051(11) -0.0059(10) 0.0057(9)
Cl01 0.0715(17) 0.0785(18) 0.0763(16) 0.0090(12) -0.0043(11) -0.0034(12)
C012 0.0342(12) 0.0429(13) 0.0594(15) 0.0044(11) 0.0078(10) -0.0022(10)
C013 0.0336(12) 0.0259(10) 0.0621(15) -0.0051(9) -0.0055(10) 0.0028(8)
C014 0.0319(12) 0.0409(12) 0.0616(15) -0.0010(11) 0.0069(10) 0.0030(10)
C015 0.0383(13) 0.0242(10) 0.0777(18) -0.0041(11) -0.0092(11) 0.0057(9)
C016 0.0387(12) 0.0242(10) 0.0655(16) 0.0034(10) -0.0079(10) -0.0050(9)
C017 0.0407(13) 0.0287(10) 0.0543(14) -0.0005(9) -0.0132(10) 0.0073(9)
C018 0.0363(12) 0.0340(11) 0.0451(12) -0.0029(9) 0.0033(9) -0.0076(9)
C019 0.0368(12) 0.0338(11) 0.0459(12) 0.0055(9) 0.0053(9) 0.0100(9)
C01A 0.0328(13) 0.0570(16) 0.0674(17) 0.0023(13) 0.0044(11) -0.0016(11)
Cl1 0.072(2) 0.0721(18) 0.0810(19) 0.0129(13) 0.0041(13) 0.0070(13)
Cl2 0.122(3) 0.092(3) 0.0794(17) -0.0166(15) 0.0356(16) -0.031(2)
C01D 0.0445(14) 0.0595(16) 0.0452(13) -0.0086(12) 0.0101(10) -0.0129(12)
C01E 0.0372(14) 0.0562(16) 0.0654(17) 0.0031(13) 0.0048(11) 0.0052(11)
C01F 0.0473(15) 0.0648(18) 0.0461(14) 0.0082(12) 0.0106(11) 0.0179(13)
C01G 0.0302(13) 0.0732(19) 0.0563(16) 0.0114(14) 0.0062(11) 0.0065(12)
C01H 0.0349(13) 0.0668(17) 0.0551(15) -0.0078(13) 0.0052(11) -0.0008(12)
Cl3 0.067(3) 0.0345(17) 0.0338(17) -0.0024(11) 0.0035(14) -0.0058(14)
Cl4 0.073(3) 0.046(3) 0.063(3) -0.0158(19) 0.043(2) -0.011(2)
Cl2A 0.067(6) 0.078(7) 0.072(6) 0.013(5) -0.017(4) -0.001(5)
Cl1A 0.081(9) 0.089(8) 0.072(7) 0.022(5) 0.020(5) 0.016(6)
Cl0A 0.140(7) 0.249(15) 0.079(3) -0.006(6) 0.050(4) -0.080(10)
_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
Co01 O007 2.0102(15) 3_656 ?
Co01 O007 2.0102(16) . ?
Co01 N009 2.2111(18) 3_656 ?
Co01 N009 2.2110(18) . ?
Co01 N00A 2.2487(18) 3_656 ?
Co01 N00A 2.2487(18) . ?
Co02 O008 2.0117(16) 3_566 ?
Co02 O008 2.0118(16) . ?
Co02 N00B 2.2340(18) 3_566 ?
Co02 N00B 2.2340(18) . ?
Co02 N00C 2.2119(18) 3_566 ?
Co02 N00C 2.2119(18) . ?
P003 O008 1.5002(17) . ?
P003 N00D 1.576(2) . ?
P003 N00H 1.6656(19) . ?
P003 N00I 1.6639(19) . ?
P004 O007 1.4990(16) . ?
P004 N00E 1.577(2) . ?
P004 N00F 1.6625(19) . ?
P004 N00G 1.6573(19) . ?
Cl05 Cl2A 1.873(10) . ?
Cl05 Cl1A 1.148(13) . ?
Cl06 Cl0A 0.77(3) . ?
N009 C00M 1.340(3) . ?
N009 C00V 1.357(3) . ?
N00A C00P 1.346(3) . ?
N00A C00Q 1.357(3) . ?
N00B C00R 1.339(3) . ?
N00B C00S 1.364(3) . ?
N00C C00O 1.337(3) . ?
N00C C013 1.356(3) . ?
N00D H00D 0.8600 . ?
N00D C019 1.335(3) . ?
N00E H00E 0.8600 . ?
N00E C018 1.333(3) . ?
N00F H00F 0.8600 . ?
N00F C00M 1.391(3) . ?
N00G H00G 0.8600 . ?
N00G C00P 1.383(3) . ?
N00H H00H 0.8600 . ?
N00H C00O 1.390(3) . ?
N00I H00I 0.8600 . ?
N00I C00R 1.384(3) . ?
N00J H00J 0.8600 . ?
N00J C019 1.362(3) . ?
N00J C01F 1.360(4) . ?
N00K H00K 0.8600 . ?
N00K C018 1.363(3) . ?
N00K C01D 1.361(4) . ?
C00L H00L 0.9300 . ?
C00L C00M 1.416(3) . ?
C00L C00T 1.377(3) . ?
C00N H00N 0.9300 . ?
C00N C00O 1.417(3) . ?
C00N C00U 1.377(4) . ?
C00P C017 1.417(3) . ?
C00Q H00Q 0.9300 . ?
C00Q C010 1.387(3) . ?
C00R C00Y 1.413(3) . ?
C00S H00S 0.9300 . ?
C00S C00X 1.379(3) . ?
C00T H00T 0.9300 . ?
C00T C016 1.390(4) . ?
C00U H00U 0.9300 . ?
C00U C015 1.385(4) . ?
C00V H00V 0.9300 . ?
C00V C016 1.384(3) . ?
C00W H00W 0.9300 . ?
C00W C00X 1.384(4) . ?
C00W C00Y 1.371(4) . ?
C00X H00X 0.9300 . ?
C00Y H00Y 0.9300 . ?
C00Z H00Z 0.9300 . ?
C00Z C010 1.383(4) . ?
C00Z C017 1.374(4) . ?
C010 H010 0.9300 . ?
Cl01 Cl3 1.941(5) . ?
Cl01 Cl1A 2.406(11) 2 ?
C012 H012 0.9300 . ?
C012 C018 1.407(4) . ?
C012 C01E 1.372(4) . ?
C013 H013 0.9300 . ?
C013 C015 1.384(3) . ?
C014 H014 0.9300 . ?
C014 C019 1.405(4) . ?
C014 C01A 1.373(4) . ?
C015 H015 0.9300 . ?
C016 H016 0.9300 . ?
C017 H017 0.9300 . ?
C01A H01A 0.9300 . ?
C01A C01G 1.404(4) . ?
Cl1 Cl3 1.173(5) . ?
Cl2 Cl4 0.982(5) . ?
C01D H01D 0.9300 . ?
C01D C01H 1.347(4) . ?
C01E H01E 0.9300 . ?
C01E C01H 1.401(4) . ?
C01F H01F 0.9300 . ?
C01F C01G 1.349(5) . ?
C01G H01G 0.9300 . ?
C01H H01H 0.9300 . ?
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
O007 Co01 O007 180.0 3_656 . ?
O007 Co01 N009 88.43(6) . . ?
O007 Co01 N009 91.57(7) . 3_656 ?
O007 Co01 N009 91.57(7) 3_656 . ?
O007 Co01 N009 88.43(6) 3_656 3_656 ?
O007 Co01 N00A 89.05(6) . . ?
O007 Co01 N00A 90.95(6) . 3_656 ?
O007 Co01 N00A 89.05(6) 3_656 3_656 ?
O007 Co01 N00A 90.95(6) 3_656 . ?
N009 Co01 N009 180.0 . 3_656 ?
N009 Co01 N00A 87.23(6) 3_656 3_656 ?
N009 Co01 N00A 92.77(6) . 3_656 ?
N009 Co01 N00A 92.77(6) 3_656 . ?
N009 Co01 N00A 87.23(6) . . ?
N00A Co01 N00A 180.00(7) . 3_656 ?
O008 Co02 O008 180.0 3_566 . ?
O008 Co02 N00B 91.04(7) 3_566 . ?
O008 Co02 N00B 88.96(7) . . ?
O008 Co02 N00B 88.96(7) 3_566 3_566 ?
O008 Co02 N00B 91.04(7) . 3_566 ?
O008 Co02 N00C 89.06(7) 3_566 3_566 ?
O008 Co02 N00C 90.94(7) 3_566 . ?
O008 Co02 N00C 89.06(7) . . ?
O008 Co02 N00C 90.94(7) . 3_566 ?
N00B Co02 N00B 180.0 3_566 . ?
N00C Co02 N00B 92.86(7) . 3_566 ?
N00C Co02 N00B 87.14(7) . . ?
N00C Co02 N00B 87.14(7) 3_566 3_566 ?
N00C Co02 N00B 92.86(7) 3_566 . ?
N00C Co02 N00C 180.0 3_566 . ?
O008 P003 N00D 120.36(10) . . ?
O008 P003 N00H 108.17(10) . . ?
O008 P003 N00I 109.07(10) . . ?
N00D P003 N00H 107.35(10) . . ?
N00D P003 N00I 101.76(11) . . ?
N00I P003 N00H 109.76(11) . . ?
O007 P004 N00E 119.80(10) . . ?
O007 P004 N00F 108.27(10) . . ?
O007 P004 N00G 109.57(10) . . ?
N00E P004 N00F 107.57(10) . . ?
N00E P004 N00G 101.29(10) . . ?
N00G P004 N00F 110.00(11) . . ?
Cl1A Cl05 Cl2A 144.2(7) . . ?
P004 O007 Co01 119.32(9) . . ?
P003 O008 Co02 119.45(9) . . ?
C00M N009 Co01 126.54(14) . . ?
C00M N009 C00V 117.00(19) . . ?
C00V N009 Co01 116.25(16) . . ?
C00P N00A Co01 128.56(14) . . ?
C00P N00A C00Q 117.16(18) . . ?
C00Q N00A Co01 113.88(15) . . ?
C00R N00B Co02 128.86(14) . . ?
C00R N00B C00S 116.85(19) . . ?
C00S N00B Co02 113.87(15) . . ?
C00O N00C Co02 126.55(14) . . ?
C00O N00C C013 117.1(2) . . ?
C013 N00C Co02 116.05(17) . . ?
P003 N00D H00D 117.3 . . ?
C019 N00D P003 125.38(18) . . ?
C019 N00D H00D 117.3 . . ?
P004 N00E H00E 117.2 . . ?
C018 N00E P004 125.57(17) . . ?
C018 N00E H00E 117.2 . . ?
P004 N00F H00F 114.2 . . ?
C00M N00F P004 131.62(17) . . ?
C00M N00F H00F 114.2 . . ?
P004 N00G H00G 116.5 . . ?
C00P N00G P004 127.01(16) . . ?
C00P N00G H00G 116.5 . . ?
P003 N00H H00H 114.2 . . ?
C00O N00H P003 131.57(17) . . ?
C00O N00H H00H 114.2 . . ?
P003 N00I H00I 116.1 . . ?
C00R N00I P003 127.76(16) . . ?
C00R N00I H00I 116.1 . . ?
C019 N00J H00J 118.1 . . ?
C01F N00J H00J 118.1 . . ?
C01F N00J C019 123.7(3) . . ?
C018 N00K H00K 117.9 . . ?
C01D N00K H00K 117.9 . . ?
C01D N00K C018 124.2(2) . . ?
C00M C00L H00L 120.4 . . ?
C00T C00L H00L 120.4 . . ?
C00T C00L C00M 119.1(2) . . ?
N009 C00M N00F 120.73(19) . . ?
N009 C00M C00L 122.5(2) . . ?
N00F C00M C00L 116.8(2) . . ?
C00O C00N H00N 120.5 . . ?
C00U C00N H00N 120.5 . . ?
C00U C00N C00O 119.0(2) . . ?
N00C C00O N00H 120.81(19) . . ?
N00C C00O C00N 122.3(2) . . ?
N00H C00O C00N 116.9(2) . . ?
N00A C00P N00G 119.47(18) . . ?
N00A C00P C017 122.2(2) . . ?
N00G C00P C017 118.3(2) . . ?
N00A C00Q H00Q 118.1 . . ?
N00A C00Q C010 123.8(2) . . ?
C010 C00Q H00Q 118.1 . . ?
N00B C00R N00I 119.53(19) . . ?
N00B C00R C00Y 122.0(2) . . ?
N00I C00R C00Y 118.5(2) . . ?
N00B C00S H00S 117.9 . . ?
N00B C00S C00X 124.3(2) . . ?
C00X C00S H00S 117.9 . . ?
C00L C00T H00T 120.5 . . ?
C00L C00T C016 118.9(2) . . ?
C016 C00T H00T 120.5 . . ?
C00N C00U H00U 120.4 . . ?
C00N C00U C015 119.1(2) . . ?
C015 C00U H00U 120.4 . . ?
N009 C00V H00V 118.0 . . ?
N009 C00V C016 123.9(2) . . ?
C016 C00V H00V 118.0 . . ?
C00X C00W H00W 120.2 . . ?
C00Y C00W H00W 120.2 . . ?
C00Y C00W C00X 119.6(2) . . ?
C00S C00X C00W 117.9(2) . . ?
C00S C00X H00X 121.1 . . ?
C00W C00X H00X 121.1 . . ?
C00R C00Y H00Y 120.4 . . ?
C00W C00Y C00R 119.3(2) . . ?
C00W C00Y H00Y 120.4 . . ?
C010 C00Z H00Z 120.1 . . ?
C017 C00Z H00Z 120.1 . . ?
C017 C00Z C010 119.9(2) . . ?
C00Q C010 H010 121.0 . . ?
C00Z C010 C00Q 118.1(2) . . ?
C00Z C010 H010 121.0 . . ?
Cl3 Cl01 Cl1A 99.7(4) . 2 ?
C018 C012 H012 119.8 . . ?
C01E C012 H012 119.8 . . ?
C01E C012 C018 120.4(2) . . ?
N00C C013 H013 118.0 . . ?
N00C C013 C015 123.9(3) . . ?
C015 C013 H013 118.0 . . ?
C019 C014 H014 119.7 . . ?
C01A C014 H014 119.7 . . ?
C01A C014 C019 120.7(3) . . ?
C00U C015 C013 118.4(2) . . ?
C00U C015 H015 120.8 . . ?
C013 C015 H015 120.8 . . ?
C00T C016 H016 120.7 . . ?
C00V C016 C00T 118.5(2) . . ?
C00V C016 H016 120.7 . . ?
C00P C017 H017 120.6 . . ?
C00Z C017 C00P 118.7(2) . . ?
C00Z C017 H017 120.6 . . ?
N00E C018 N00K 116.0(2) . . ?
N00E C018 C012 128.1(2) . . ?
N00K C018 C012 115.8(2) . . ?
N00D C019 N00J 115.6(2) . . ?
N00D C019 C014 128.3(2) . . ?
N00J C019 C014 116.1(2) . . ?
C014 C01A H01A 119.7 . . ?
C014 C01A C01G 120.6(3) . . ?
C01G C01A H01A 119.7 . . ?
N00K C01D H01D 119.8 . . ?
C01H C01D N00K 120.4(3) . . ?
C01H C01D H01D 119.8 . . ?
C012 C01E H01E 119.4 . . ?
C012 C01E C01H 121.2(3) . . ?
C01H C01E H01E 119.4 . . ?
N00J C01F H01F 119.6 . . ?
C01G C01F N00J 120.7(3) . . ?
C01G C01F H01F 119.6 . . ?
C01A C01G H01G 120.9 . . ?
C01F C01G C01A 118.1(3) . . ?
C01F C01G H01G 120.9 . . ?
C01D C01H C01E 118.0(3) . . ?
C01D C01H H01H 121.0 . . ?
C01E C01H H01H 121.0 . . ?
Cl1 Cl3 Cl01 148.3(3) . . ?
Cl05 Cl1A Cl01 125.7(8) . 2_545 ?
_iucr_refine_instructions_details
;
TITL ms3k_c2_a.res in P2(1)/n
ms3k_c2.res
created by SHELXL-2018/1 at 17:12:43 on 24-Jul-2019
REM Old TITL ms3k_c2_a.res in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.172, Rweak 0.001, Alpha 0.035, Orientation as input
REM Formula found by SHELXT: C35 N10 O4 P2 Cl2 Co
CELL 0.7 8.513 15.816 26.981 90 93.058 90
ZERR 27 0.0017 0.0032 0.0054 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O P Cl Co
DISP C 0.0033 0.0016 11.1819
DISP Cl 0.1453 0.1556 651.6741
DISP Co 0.3554 0.9393 3858.4229
DISP H -0 0 0.6234
DISP N 0.0063 0.0031 18.9823
DISP O 0.0112 0.0059 31.3712
DISP P 0.1018 0.0938 394.0833
UNIT 27 27 27 27 27 27 27
SUMP 3 0.01 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11
SUMP 3 0.01 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11
L.S. 10
PLAN 20
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.082100 3.176100
EXTI 0.009567
FVAR 0.34641 0.36053 0.18037 0.33122 0.46057 0.32005 0.39803
FVAR 0.17182 0.08702 0.65421 0.08934
CO01 7 0.500000 0.000000 0.500000 10.50000 0.01893 0.02198 =
0.04059 0.00219 -0.00144 -0.00054
CO02 7 0.000000 0.500000 0.500000 10.50000 0.01835 0.02165 =
0.04656 -0.00254 -0.00145 0.00076
P003 5 0.102786 0.451794 0.397423 11.00000 0.02653 0.02291 =
0.04668 0.00073 0.00272 0.00038
P004 5 0.614938 0.048980 0.399189 11.00000 0.02747 0.02373 =
0.04193 0.00068 0.00252 -0.00028
CL05 6 0.606000 -0.227713 0.212769 101.00000 0.05141 0.03328 =
0.04548 -0.00244 0.00775 0.00017
CL06 6 0.378856 0.109066 0.225440 51.00000 0.04484 0.03510 =
0.04564 -0.01220 0.01875 -0.00932
O007 4 0.660796 0.039933 0.453345 11.00000 0.02285 0.02987 =
0.04437 0.00318 -0.00001 -0.00460
O008 4 0.153316 0.457888 0.451427 11.00000 0.02388 0.02975 =
0.04849 -0.00405 -0.00055 0.00405
N009 3 0.447725 -0.107072 0.449071 11.00000 0.02320 0.02120 =
0.04847 0.00122 -0.00376 0.00154
N00A 3 0.315385 0.073367 0.455505 11.00000 0.02350 0.02411 =
0.04509 -0.00237 -0.00502 0.00174
N00B 3 -0.190999 0.429533 0.457693 11.00000 0.02280 0.02375 =
0.05058 0.00215 -0.00469 -0.00154
N00C 3 -0.055118 0.608198 0.450116 11.00000 0.02204 0.02116 =
0.05584 -0.00073 -0.00407 -0.00079
N00D 3 0.219167 0.416490 0.358917 11.00000 0.03633 0.02883 =
0.05095 -0.00213 0.00813 0.00086
AFIX 43
H00D 2 0.193715 0.369970 0.344065 11.00000 -1.20000
AFIX 0
N00E 3 0.738263 0.083293 0.362524 11.00000 0.03760 0.02857 =
0.04714 0.00299 0.00798 -0.00236
AFIX 43
H00E 2 0.720049 0.132035 0.349307 11.00000 -1.20000
AFIX 0
N00F 3 0.552203 -0.044427 0.377938 11.00000 0.03430 0.02915 =
0.04534 -0.00542 0.00668 -0.00429
AFIX 43
H00F 2 0.571024 -0.053750 0.347418 11.00000 -1.20000
AFIX 0
N00G 3 0.472745 0.120127 0.391656 11.00000 0.03929 0.03164 =
0.04355 0.00616 0.00354 0.00949
AFIX 43
H00G 2 0.487683 0.160037 0.370776 11.00000 -1.20000
AFIX 0
N00H 3 0.045406 0.547425 0.377972 11.00000 0.03296 0.02840 =
0.05312 0.00794 0.00814 0.00412
AFIX 43
H00H 2 0.067172 0.558642 0.347913 11.00000 -1.20000
AFIX 0
N00I 3 -0.046717 0.384285 0.390601 11.00000 0.03940 0.02947 =
0.04377 -0.00304 0.00160 -0.00807
AFIX 43
H00I 2 -0.039124 0.346336 0.368026 11.00000 -1.20000
AFIX 0
N00J 3 0.430370 0.415039 0.310289 11.00000 0.04946 0.04652 =
0.04443 0.00365 0.01115 0.00787
AFIX 43
H00J 2 0.386912 0.371864 0.295847 11.00000 -1.20000
AFIX 0
N00K 3 0.950918 0.080387 0.314235 11.00000 0.04857 0.04218 =
0.04479 -0.00223 0.01011 -0.00554
AFIX 43
H00K 2 0.913771 0.126111 0.300937 11.00000 -1.20000
AFIX 0
C00L 1 0.426878 -0.179414 0.370107 11.00000 0.03265 0.02862 =
0.05401 -0.00677 -0.00161 0.00384
AFIX 43
H00L 2 0.450781 -0.180729 0.336882 11.00000 -1.20000
AFIX 0
C00M 1 0.474745 -0.110239 0.400619 11.00000 0.02114 0.02327 =
0.05259 -0.00217 -0.00131 0.00265
C00N 1 -0.082817 0.681825 0.371807 11.00000 0.03307 0.02920 =
0.06208 0.00878 -0.00144 -0.00240
AFIX 43
H00N 2 -0.061495 0.683948 0.338381 11.00000 -1.20000
AFIX 0
C00O 1 -0.031325 0.612348 0.401589 11.00000 0.02054 0.02268 =
0.06064 0.00398 -0.00036 -0.00227
C00P 1 0.332624 0.122235 0.415333 11.00000 0.03254 0.02360 =
0.04324 -0.00388 -0.00721 0.00360
C00Q 1 0.172931 0.074351 0.475786 11.00000 0.02395 0.03188 =
0.05567 -0.00049 -0.00253 0.00283
AFIX 43
H00Q 2 0.158496 0.039746 0.503037 11.00000 -1.20000
AFIX 0
C00R 1 -0.181786 0.381906 0.416905 11.00000 0.03050 0.02286 =
0.04665 0.00504 -0.00595 -0.00259
C00S 1 -0.330573 0.428555 0.480307 11.00000 0.02282 0.03120 =
0.05897 0.00083 -0.00159 -0.00075
AFIX 43
H00S 2 -0.339739 0.462475 0.508160 11.00000 -1.20000
AFIX 0
C00T 1 0.344482 -0.244695 0.390285 11.00000 0.03569 0.02414 =
0.06821 -0.00602 -0.00791 -0.00024
AFIX 43
H00T 2 0.309565 -0.290051 0.370719 11.00000 -1.20000
AFIX 0
C00U 1 -0.164926 0.746176 0.393102 11.00000 0.03589 0.02354 =
0.08151 0.00819 -0.00811 0.00228
AFIX 43
H00U 2 -0.202323 0.791617 0.374041 11.00000 -1.20000
AFIX 0
C00V 1 0.369560 -0.173306 0.468133 11.00000 0.03287 0.02479 =
0.05380 0.00480 -0.00392 -0.00242
AFIX 43
H00V 2 0.352069 -0.172687 0.501862 11.00000 -1.20000
AFIX 0
C00W 1 -0.444407 0.329010 0.423614 11.00000 0.03032 0.02918 =
0.06788 0.00662 -0.01166 -0.00863
AFIX 43
H00W 2 -0.527674 0.294675 0.412480 11.00000 -1.20000
AFIX 0
C00X 1 -0.458892 0.380563 0.464558 11.00000 0.02409 0.03486 =
0.07067 0.00504 -0.00401 -0.00369
AFIX 43
H00X 2 -0.552215 0.382763 0.480929 11.00000 -1.20000
AFIX 0
C00Y 1 -0.306518 0.328864 0.399558 11.00000 0.03910 0.02757 =
0.05431 0.00308 -0.00997 -0.00702
AFIX 43
H00Y 2 -0.295205 0.294231 0.372122 11.00000 -1.20000
AFIX 0
C00Z 1 0.069876 0.176561 0.418305 11.00000 0.03481 0.03056 =
0.06779 -0.00494 -0.01656 0.01001
AFIX 43
H00Z 2 -0.010877 0.211931 0.406416 11.00000 -1.20000
AFIX 0
C010 1 0.047541 0.123961 0.458250 11.00000 0.02627 0.03538 =
0.07198 -0.00514 -0.00589 0.00567
AFIX 43
H010 2 -0.048757 0.121892 0.472940 11.00000 -1.20000
AFIX 0
CL01 6 0.242908 0.293649 0.248965 21.00000 0.07148 0.07849 =
0.07626 0.00900 -0.00432 -0.00344
C012 1 0.934424 -0.031092 0.371147 11.00000 0.03424 0.04294 =
0.05936 0.00442 0.00781 -0.00223
AFIX 43
H012 2 0.884517 -0.058768 0.396339 11.00000 -1.20000
AFIX 0
C013 1 -0.133046 0.673521 0.470168 11.00000 0.03355 0.02588 =
0.06210 -0.00511 -0.00545 0.00281
AFIX 43
H013 2 -0.148433 0.672008 0.504024 11.00000 -1.20000
AFIX 0
C014 1 0.429060 0.523365 0.369776 11.00000 0.03186 0.04086 =
0.06158 -0.00097 0.00693 0.00296
AFIX 43
H014 2 0.382315 0.551346 0.395487 11.00000 -1.20000
AFIX 0
C015 1 -0.191057 0.742299 0.443296 11.00000 0.03833 0.02423 =
0.07773 -0.00414 -0.00924 0.00566
AFIX 43
H015 2 -0.246253 0.784895 0.458560 11.00000 -1.20000
AFIX 0
C016 1 0.314325 -0.241707 0.440388 11.00000 0.03869 0.02415 =
0.06553 0.00343 -0.00790 -0.00499
AFIX 43
H016 2 0.258263 -0.284734 0.454935 11.00000 -1.20000
AFIX 0
C017 1 0.211612 0.176479 0.396207 11.00000 0.04069 0.02873 =
0.05431 -0.00050 -0.01319 0.00726
AFIX 43
H017 2 0.227791 0.211371 0.369208 11.00000 -1.20000
AFIX 0
C018 1 0.868335 0.043203 0.350265 11.00000 0.03628 0.03404 =
0.04507 -0.00287 0.00330 -0.00758
C019 1 0.354034 0.452840 0.347446 11.00000 0.03681 0.03383 =
0.04586 0.00550 0.00533 0.01001
C01A 1 0.570643 0.551397 0.354034 11.00000 0.03283 0.05699 =
0.06742 0.00226 0.00439 -0.00164
AFIX 43
H01A 2 0.618586 0.598358 0.369058 11.00000 -1.20000
AFIX 0
CL1 6 0.527885 0.222557 0.304634 41.00000 0.07155 0.07209 =
0.08099 0.01290 0.00415 0.00697
CL2 6 0.581804 -0.052630 0.272231 71.00000 0.12151 0.09216 =
0.07942 -0.01659 0.03557 -0.03075
C01D 1 1.088368 0.049769 0.297973 11.00000 0.04451 0.05948 =
0.04525 -0.00859 0.01012 -0.01292
AFIX 43
H01D 2 1.139494 0.078710 0.273519 11.00000 -1.20000
AFIX 0
C01E 1 1.072024 -0.062922 0.354558 11.00000 0.03722 0.05622 =
0.06541 0.00308 0.00481 0.00519
AFIX 43
H01E 2 1.113685 -0.112414 0.368454 11.00000 -1.20000
AFIX 0
C01F 1 0.571400 0.441669 0.294720 11.00000 0.04727 0.06480 =
0.04613 0.00816 0.01059 0.01793
AFIX 43
H01F 2 0.618455 0.412554 0.269492 11.00000 -1.20000
AFIX 0
C01G 1 0.643769 0.509843 0.315465 11.00000 0.03024 0.07323 =
0.05625 0.01140 0.00620 0.00646
AFIX 43
H01G 2 0.739383 0.528793 0.304538 11.00000 -1.20000
AFIX 0
C01H 1 1.150879 -0.022178 0.317054 11.00000 0.03495 0.06684 =
0.05515 -0.00785 0.00519 -0.00079
AFIX 43
H01H 2 1.243654 -0.044159 0.305669 11.00000 -1.20000
AFIX 0
CL3 6 0.399193 0.227744 0.287091 31.00000 0.06701 0.03448 =
0.03384 -0.00237 0.00352 -0.00582
CL4 6 0.622726 -0.110551 0.275021 81.00000 0.07315 0.04574 =
0.06342 -0.01579 0.04303 -0.01098
CL2A 6 0.749452 -0.293682 0.250998 111.00000 0.06665 0.07841 =
0.07207 0.01267 -0.01691 -0.00133
CL1A 6 0.476445 -0.221504 0.199096 91.00000 0.08137 0.08925 =
0.07230 0.02185 0.01977 0.01576
CL0A 6 0.425250 0.069200 0.233599 61.00000 0.14034 0.24889 =
0.07908 -0.00581 0.05001 -0.07964
HKLF 4
REM ms3k_c2_a.res in P2(1)/n
REM R1 = 0.0492 for 7105 Fo > 4sig(Fo) and 0.0576 for all 8709 data
REM 528 parameters refined using 2 restraints
END
WGHT 0.0822 3.0361
REM Highest difference peak 0.936, deepest hole -0.670, 1-sigma level 0.091
Q1 1 0.4430 0.1130 0.2484 11.00000 0.05 0.94
Q2 1 0.5124 0.1826 0.2867 11.00000 0.05 0.84
Q3 1 0.5592 -0.1039 0.2498 11.00000 0.05 0.82
Q4 1 0.5094 0.0012 0.2527 11.00000 0.05 0.71
Q5 1 0.5490 -0.1821 0.2099 11.00000 0.05 0.64
Q6 1 0.6324 0.2187 0.2958 11.00000 0.05 0.54
Q7 1 0.4782 0.0555 0.2274 11.00000 0.05 0.51
Q8 1 0.4675 -0.1816 0.2138 11.00000 0.05 0.51
Q9 1 0.7846 -0.2959 0.2156 11.00000 0.05 0.48
Q10 1 0.2812 0.3165 0.2738 11.00000 0.05 0.47
Q11 1 0.1548 0.2824 0.2660 11.00000 0.05 0.44
Q12 1 0.3339 0.2609 0.2651 11.00000 0.05 0.43
Q13 1 0.4976 0.0052 0.4638 11.00000 0.05 0.42
Q14 1 0.5194 -0.0610 0.2747 11.00000 0.05 0.42
Q15 1 0.1113 0.4631 0.4305 11.00000 0.05 0.41
Q16 1 0.2781 0.2573 0.2368 11.00000 0.05 0.41
Q17 1 0.3456 0.1365 0.2229 11.00000 0.05 0.41
Q18 1 0.6737 -0.0762 0.2837 11.00000 0.05 0.37
Q19 1 0.5215 0.0840 0.3900 11.00000 0.05 0.36
Q20 1 0.0167 0.4164 0.3925 11.00000 0.05 0.35
REM The information below was added by Olex2.
REM
REM R1 = 0.0492 for 7105 Fo > 4sig(Fo) and 0.0576 for all 52489 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.94, deepest hole -0.67
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0576
REM R1_gt = 0.0492
REM wR_ref = 0.1598
REM GOOF = 1.037
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 52489
REM Reflections_gt = 7105
REM Parameters = n/a
REM Hole = -0.67
REM Peak = 0.94
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_ms1k_c3
_database_code_depnum_ccdc_archive 'CCDC 1956239'
loop_
_audit_author_name
_audit_author_address
'Dan G Dumitrescu'
;Sincrotrone Elettra Trieste
Italy
;
_audit_update_record
;
2019-09-26 deposited with the CCDC. 2021-02-01 downloaded from the CCDC.
;
_audit_creation_date 2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C15 H15 N6 O P), 2(C3 H7 N O), H2 O'
_chemical_formula_sum 'C36 H46 N14 O5 P2'
_chemical_formula_weight 816.81
_chemical_melting_point ?
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'
N N 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.625(2)
_cell_length_b 18.707(4)
_cell_length_c 20.479(4)
_cell_angle_alpha 90
_cell_angle_beta 98.25(3)
_cell_angle_gamma 90
_cell_volume 4028.3(14)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 52157
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.667
_cell_measurement_theta_min 1.459
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.160
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.347
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1720
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0318
_diffrn_reflns_av_unetI/netI 0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 57512
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 24.835
_diffrn_reflns_theta_max 27.667
_diffrn_reflns_theta_min 1.459
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Arinax MD2S/Pilatus 6M'
_diffrn_measurement_method 'rotating crystal'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.700
_diffrn_source SCW
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9586
_reflns_number_total 9811
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.630
_refine_diff_density_min -0.768
_refine_diff_density_rms 0.084
_refine_ls_extinction_coef 0.0765(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 522
_refine_ls_number_reflns 9811
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0402
_refine_ls_R_factor_gt 0.0399
_refine_ls_restrained_S_all 1.060
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.0043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1065
_refine_ls_wR_factor_ref 0.1069
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
N007(H007), N00A(H00A)
2.b Free rotating group:
O006(H00B,H00D)
2.c Aromatic/amide H refined with riding coordinates:
N008(H008), N009(H009), N00C(H00C), N00G(H00G), C00S(H00S), C00T(H00T),
C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01N), C01H(H01H)
2.d Idealised Me refined as rotating group:
C01I(H01O,H01P,H01Q), C01J(H01R,H01S,H01T), C01K(H01G,H01I,H01J), C01L(H01K,
H01L,H01M)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
P001 P 0.45656(3) 0.88162(2) 0.47704(2) 0.01328(8) Uani 1 1 d . . . . .
P002 P 0.75353(3) 0.65654(2) 0.45107(2) 0.01559(9) Uani 1 1 d . . . . .
O003 O 0.38888(8) 0.93238(4) 0.51550(4) 0.01693(16) Uani 1 1 d . . . . .
O004 O 0.97919(9) 0.70101(6) 0.33141(5) 0.0291(2) Uani 1 1 d . . . . .
O005 O 0.78675(8) 0.59272(5) 0.41461(4) 0.02123(18) Uani 1 1 d . . . . .
O006 O 0.66870(11) 0.50499(5) 0.31460(5) 0.0324(2) Uani 1 1 d . . . . .
H00B H 0.700162 0.531012 0.346886 0.049 Uiso 1 1 d G . . . .
H00D H 0.648443 0.534262 0.283096 0.049 Uiso 1 1 d G . . . .
N007 N 0.75212(9) 0.64232(5) 0.53032(5) 0.01725(19) Uani 1 1 d . . . . .
H007 H 0.732374 0.681630 0.548120 0.021 Uiso 1 1 d R . . . .
N008 N 0.52153(9) 0.81207(5) 0.51871(5) 0.01529(18) Uani 1 1 d . . . . .
H008 H 0.602957 0.808665 0.522368 0.018 Uiso 1 1 calc R . . . .
N009 N 0.60982(9) 0.68922(5) 0.42597(5) 0.01637(19) Uani 1 1 d . . . . .
H009 H 0.605404 0.733665 0.415169 0.020 Uiso 1 1 calc R . . . .
N00A N 0.36195(9) 0.84525(5) 0.41534(5) 0.01562(18) Uani 1 1 d . . . . .
H00A H 0.405669 0.815587 0.395657 0.019 Uiso 1 1 d R . . . .
N00B N 0.63397(10) 0.83784(5) 0.37703(5) 0.01755(19) Uani 1 1 d . . . . .
N00C N 0.57730(9) 0.92354(5) 0.45154(5) 0.01597(18) Uani 1 1 d . . . . .
H00C H 0.598113 0.963571 0.470766 0.019 Uiso 1 1 calc R . . . .
N00D N 0.53490(10) 0.70652(5) 0.57717(5) 0.0184(2) Uani 1 1 d . . . . .
N00E N 0.80732(9) 0.80619(5) 0.51757(5) 0.0185(2) Uani 1 1 d . . . . .
N00F N 0.39105(9) 0.69177(5) 0.40365(5) 0.01703(19) Uani 1 1 d . . . . .
N00G N 0.85446(9) 0.72115(5) 0.44010(5) 0.01774(19) Uani 1 1 d . . . . .
H00G H 0.894720 0.715194 0.406955 0.021 Uiso 1 1 calc R . . . .
N00H N 0.81916(10) 0.60356(6) 0.63602(5) 0.0219(2) Uani 1 1 d . . . . .
O00I O 0.60142(12) 0.60543(6) 0.21598(5) 0.0374(3) Uani 1 1 d . . . . .
N00J N 0.49173(11) 0.71009(6) 0.21490(6) 0.0265(2) Uani 1 1 d . . . . .
N00K N 0.98182(11) 0.64158(6) 0.23480(5) 0.0250(2) Uani 1 1 d . . . . .
N00L N 0.21119(10) 0.83859(6) 0.32309(6) 0.0232(2) Uani 1 1 d . . . . .
C00M C 0.49498(11) 0.65168(6) 0.42061(5) 0.0157(2) Uani 1 1 d . . . . .
C00N C 0.45892(11) 0.75806(6) 0.54871(5) 0.0155(2) Uani 1 1 d . . . . .
C00O C 0.65043(10) 0.90319(6) 0.40317(5) 0.0154(2) Uani 1 1 d . . . . .
C00P C 0.84577(11) 0.60770(6) 0.57432(6) 0.0175(2) Uani 1 1 d . . . . .
C00Q C 0.88493(10) 0.78369(6) 0.47582(6) 0.0168(2) Uani 1 1 d . . . . .
C00R C 0.27826(10) 0.88136(6) 0.36754(5) 0.0160(2) Uani 1 1 d . . . . .
C00S C 0.32679(11) 0.75724(6) 0.54779(6) 0.0201(2) Uani 1 1 d . . . . .
H00S H 0.276265 0.794599 0.529043 0.024 Uiso 1 1 calc R . . . .
C00T C 0.70351(12) 0.82080(7) 0.32890(6) 0.0203(2) Uani 1 1 d . . . . .
H00T H 0.692201 0.775715 0.309830 0.024 Uiso 1 1 calc R . . . .
C00U C 0.80893(12) 0.93328(7) 0.33578(6) 0.0236(2) Uani 1 1 d . . . . .
H00U H 0.868070 0.964802 0.322544 0.028 Uiso 1 1 calc R . . . .
C00V C 0.99611(11) 0.82084(7) 0.46584(6) 0.0210(2) Uani 1 1 d . . . . .
H00V H 1.047317 0.804176 0.435895 0.025 Uiso 1 1 calc R . . . .
C00W C 0.26571(13) 0.95584(7) 0.36623(6) 0.0232(2) Uani 1 1 d . . . . .
H00W H 0.313382 0.984276 0.397862 0.028 Uiso 1 1 calc R . . . .
C00X C 0.95653(11) 0.57933(6) 0.55460(6) 0.0211(2) Uani 1 1 d . . . . .
H00X H 0.970925 0.582169 0.510939 0.025 Uiso 1 1 calc R . . . .
C00Y C 0.90584(13) 0.57153(7) 0.68109(7) 0.0263(3) Uani 1 1 d . . . . .
H00Y H 0.888360 0.568155 0.724203 0.032 Uiso 1 1 calc R . . . .
C00Z C 0.27665(11) 0.65956(6) 0.39669(6) 0.0211(2) Uani 1 1 d . . . . .
H00Z H 0.204477 0.687434 0.384955 0.025 Uiso 1 1 calc R . . . .
C010 C 0.84116(12) 0.86622(7) 0.55230(6) 0.0214(2) Uani 1 1 d . . . . .
H010 H 0.788691 0.881887 0.582036 0.026 Uiso 1 1 calc R . . . .
C011 C 0.17993(13) 0.98598(7) 0.31628(6) 0.0262(3) Uani 1 1 d . . . . .
H011 H 0.169093 1.035301 0.314311 0.031 Uiso 1 1 calc R . . . .
C012 C 0.27379(13) 0.69915(7) 0.57562(7) 0.0249(3) Uani 1 1 d . . . . .
H012 H 0.186041 0.696089 0.574055 0.030 Uiso 1 1 calc R . . . .
C013 C 0.73876(11) 0.95241(6) 0.38476(6) 0.0190(2) Uani 1 1 d . . . . .
H013 H 0.749710 0.996868 0.405110 0.023 Uiso 1 1 calc R . . . .
C014 C 1.01940(13) 0.54335(7) 0.66703(7) 0.0273(3) Uani 1 1 d . . . . .
H014 H 1.077518 0.522656 0.699890 0.033 Uiso 1 1 calc R . . . .
C015 C 0.79013(12) 0.86607(7) 0.30632(6) 0.0238(2) Uani 1 1 d . . . . .
H015 H 0.834701 0.852274 0.272493 0.029 Uiso 1 1 calc R . . . .
C016 C 0.48078(13) 0.65158(7) 0.60542(6) 0.0234(2) Uani 1 1 d . . . . .
H016 H 0.533501 0.615906 0.625692 0.028 Uiso 1 1 calc R . . . .
C017 C 1.04379(12) 0.54697(7) 0.60220(7) 0.0249(3) Uani 1 1 d . . . . .
H017 H 1.118403 0.527728 0.590856 0.030 Uiso 1 1 calc R . . . .
C018 C 0.94889(12) 0.90595(7) 0.54651(7) 0.0246(3) Uani 1 1 d . . . . .
H018 H 0.968478 0.946863 0.571716 0.030 Uiso 1 1 calc R . . . .
C019 C 0.26103(12) 0.58699(7) 0.40614(7) 0.0263(3) Uani 1 1 d . . . . .
H019 H 0.180540 0.566411 0.400969 0.032 Uiso 1 1 calc R . . . .
C01A C 1.02718(12) 0.88259(7) 0.50158(7) 0.0243(3) Uani 1 1 d . . . . .
H01A H 1.099597 0.908352 0.495761 0.029 Uiso 1 1 calc R . . . .
C01B C 0.11043(13) 0.94274(8) 0.26937(6) 0.0264(3) Uani 1 1 d . . . . .
H01B H 0.053183 0.961978 0.235288 0.032 Uiso 1 1 calc R . . . .
C01C C 0.35161(14) 0.64533(7) 0.60594(7) 0.0269(3) Uani 1 1 d . . . . .
H01C H 0.317724 0.606517 0.625838 0.032 Uiso 1 1 calc R . . . .
C01D C 0.93144(12) 0.65892(7) 0.28861(7) 0.0250(3) Uani 1 1 d . . . . .
H01D H 0.854596 0.637697 0.294274 0.030 Uiso 1 1 calc R . . . .
C01E C 0.48871(12) 0.57767(6) 0.43119(7) 0.0224(2) Uani 1 1 d . . . . .
H01E H 0.562185 0.550859 0.442910 0.027 Uiso 1 1 calc R . . . .
C01F C 0.12967(13) 0.86988(8) 0.27530(7) 0.0286(3) Uani 1 1 d . . . . .
H01F H 0.083085 0.840465 0.244115 0.034 Uiso 1 1 calc R . . . .
C01G C 0.52282(14) 0.64451(8) 0.23701(7) 0.0288(3) Uani 1 1 d . . . . .
H01N H 0.482092 0.626860 0.270924 0.035 Uiso 1 1 calc R . . . .
C01H C 0.36995(13) 0.54583(7) 0.42366(7) 0.0273(3) Uani 1 1 d . . . . .
H01H H 0.362824 0.496906 0.430294 0.033 Uiso 1 1 calc R . . . .
C01I C 0.55382(15) 0.74243(8) 0.16345(7) 0.0301(3) Uani 1 1 d . . . . .
H01O H 0.616246 0.710022 0.150955 0.045 Uiso 1 1 calc GR . . . .
H01P H 0.594622 0.786029 0.179613 0.045 Uiso 1 1 calc GR . . . .
H01Q H 0.491623 0.752602 0.125786 0.045 Uiso 1 1 calc GR . . . .
C01J C 0.39983(14) 0.75374(8) 0.24305(7) 0.0315(3) Uani 1 1 d . . . . .
H01R H 0.331909 0.766831 0.209040 0.047 Uiso 1 1 calc GR . . . .
H01S H 0.440822 0.796142 0.262044 0.047 Uiso 1 1 calc GR . . . .
H01T H 0.366093 0.727069 0.276643 0.047 Uiso 1 1 calc GR . . . .
C01K C 0.92090(17) 0.58985(9) 0.18735(7) 0.0368(3) Uani 1 1 d . . . . .
H01G H 0.973302 0.547989 0.187868 0.055 Uiso 1 1 calc GR . . . .
H01I H 0.909759 0.610535 0.144008 0.055 Uiso 1 1 calc GR . . . .
H01J H 0.839480 0.576912 0.198897 0.055 Uiso 1 1 calc GR . . . .
C01L C 1.10433(14) 0.67043(9) 0.22413(7) 0.0319(3) Uani 1 1 d . . . . .
H01K H 1.130199 0.706747 0.256401 0.048 Uiso 1 1 calc GR . . . .
H01L H 1.097245 0.690785 0.180729 0.048 Uiso 1 1 calc GR . . . .
H01M H 1.166412 0.632809 0.228234 0.048 Uiso 1 1 calc GR . . . .
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
P001 0.01464(14) 0.01026(13) 0.01504(14) -0.00020(9) 0.00242(10) 0.00044(9)
P002 0.01485(14) 0.01393(14) 0.01749(14) -0.00282(10) 0.00056(10) 0.00199(9)
O003 0.0186(4) 0.0131(4) 0.0199(4) -0.0017(3) 0.0053(3) 0.0010(3)
O004 0.0252(5) 0.0343(5) 0.0291(5) -0.0128(4) 0.0088(4) -0.0051(4)
O005 0.0221(4) 0.0168(4) 0.0241(4) -0.0064(3) 0.0010(3) 0.0035(3)
O006 0.0405(6) 0.0236(5) 0.0296(5) -0.0026(4) -0.0074(4) 0.0000(4)
N007 0.0172(4) 0.0153(4) 0.0188(4) -0.0005(3) 0.0009(3) 0.0041(3)
N008 0.0139(4) 0.0133(4) 0.0186(4) 0.0017(3) 0.0021(3) 0.0008(3)
N009 0.0157(4) 0.0121(4) 0.0206(4) 0.0003(3) 0.0004(3) 0.0003(3)
N00A 0.0169(4) 0.0119(4) 0.0175(4) -0.0007(3) 0.0003(3) 0.0017(3)
N00B 0.0195(5) 0.0153(4) 0.0182(4) -0.0010(3) 0.0038(4) 0.0003(3)
N00C 0.0185(4) 0.0114(4) 0.0188(4) -0.0018(3) 0.0055(3) -0.0017(3)
N00D 0.0219(5) 0.0164(4) 0.0173(4) 0.0021(3) 0.0043(4) 0.0033(4)
N00E 0.0176(4) 0.0185(5) 0.0193(4) -0.0031(4) 0.0016(4) 0.0010(4)
N00F 0.0167(4) 0.0156(4) 0.0182(4) -0.0009(3) 0.0004(3) 0.0009(3)
N00G 0.0167(4) 0.0183(5) 0.0187(4) -0.0044(4) 0.0044(3) -0.0004(3)
N00H 0.0211(5) 0.0215(5) 0.0225(5) 0.0021(4) 0.0012(4) 0.0021(4)
O00I 0.0495(7) 0.0308(5) 0.0311(5) 0.0009(4) 0.0032(5) 0.0056(5)
N00J 0.0302(6) 0.0268(5) 0.0231(5) 0.0020(4) 0.0058(4) -0.0043(4)
N00K 0.0288(6) 0.0252(5) 0.0211(5) -0.0035(4) 0.0042(4) -0.0044(4)
N00L 0.0212(5) 0.0202(5) 0.0262(5) -0.0023(4) -0.0033(4) 0.0013(4)
C00M 0.0168(5) 0.0144(5) 0.0156(5) -0.0012(4) 0.0011(4) -0.0003(4)
C00N 0.0191(5) 0.0136(5) 0.0142(5) -0.0004(4) 0.0038(4) 0.0007(4)
C00O 0.0162(5) 0.0145(5) 0.0154(5) 0.0016(4) 0.0020(4) 0.0015(4)
C00P 0.0164(5) 0.0131(5) 0.0218(5) 0.0000(4) -0.0011(4) -0.0002(4)
C00Q 0.0156(5) 0.0163(5) 0.0179(5) -0.0009(4) -0.0002(4) 0.0008(4)
C00R 0.0150(5) 0.0160(5) 0.0172(5) 0.0008(4) 0.0034(4) 0.0020(4)
C00S 0.0191(5) 0.0194(5) 0.0227(5) 0.0015(4) 0.0060(4) 0.0019(4)
C00T 0.0234(6) 0.0195(5) 0.0183(5) -0.0022(4) 0.0038(4) 0.0018(4)
C00U 0.0243(6) 0.0230(6) 0.0251(6) 0.0051(5) 0.0091(5) -0.0015(5)
C00V 0.0176(5) 0.0219(6) 0.0235(6) -0.0010(4) 0.0031(4) -0.0006(4)
C00W 0.0306(6) 0.0162(5) 0.0211(5) -0.0002(4) -0.0017(5) 0.0033(4)
C00X 0.0189(5) 0.0191(5) 0.0245(6) -0.0023(4) 0.0005(4) 0.0020(4)
C00Y 0.0275(6) 0.0265(6) 0.0236(6) 0.0044(5) -0.0008(5) 0.0019(5)
C00Z 0.0166(5) 0.0205(6) 0.0254(6) -0.0030(4) 0.0009(4) -0.0002(4)
C010 0.0223(6) 0.0203(5) 0.0214(5) -0.0047(4) 0.0018(4) 0.0016(4)
C011 0.0342(7) 0.0204(6) 0.0233(6) 0.0032(5) 0.0018(5) 0.0089(5)
C012 0.0241(6) 0.0247(6) 0.0283(6) -0.0007(5) 0.0117(5) -0.0032(5)
C013 0.0207(5) 0.0151(5) 0.0217(5) 0.0023(4) 0.0042(4) -0.0002(4)
C014 0.0240(6) 0.0247(6) 0.0302(6) 0.0039(5) -0.0060(5) 0.0038(5)
C015 0.0260(6) 0.0274(6) 0.0199(5) 0.0006(5) 0.0092(5) 0.0022(5)
C016 0.0331(7) 0.0167(5) 0.0215(6) 0.0042(4) 0.0079(5) 0.0038(5)
C017 0.0181(5) 0.0212(6) 0.0337(7) -0.0017(5) -0.0022(5) 0.0042(4)
C018 0.0254(6) 0.0198(6) 0.0271(6) -0.0060(5) -0.0015(5) -0.0025(5)
C019 0.0203(6) 0.0222(6) 0.0362(7) -0.0034(5) 0.0028(5) -0.0060(5)
C01A 0.0202(6) 0.0214(6) 0.0304(6) -0.0012(5) 0.0010(5) -0.0044(4)
C01B 0.0242(6) 0.0323(7) 0.0214(6) 0.0018(5) -0.0011(5) 0.0108(5)
C01C 0.0354(7) 0.0196(6) 0.0282(6) 0.0039(5) 0.0138(5) -0.0032(5)
C01D 0.0222(6) 0.0278(6) 0.0257(6) -0.0039(5) 0.0056(5) -0.0038(5)
C01E 0.0211(5) 0.0148(5) 0.0305(6) 0.0013(4) 0.0011(5) 0.0008(4)
C01F 0.0249(6) 0.0298(7) 0.0279(6) -0.0047(5) -0.0070(5) 0.0034(5)
C01G 0.0342(7) 0.0280(6) 0.0232(6) 0.0003(5) 0.0005(5) -0.0059(5)
C01H 0.0273(6) 0.0150(5) 0.0393(7) 0.0005(5) 0.0036(5) -0.0038(5)
C01I 0.0382(7) 0.0276(6) 0.0262(6) 0.0017(5) 0.0100(5) -0.0042(5)
C01J 0.0289(7) 0.0360(7) 0.0306(7) 0.0043(6) 0.0081(5) 0.0001(6)
C01K 0.0482(9) 0.0380(8) 0.0244(6) -0.0107(6) 0.0052(6) -0.0105(7)
C01L 0.0323(7) 0.0377(7) 0.0279(7) -0.0026(6) 0.0119(5) -0.0045(6)
_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
P001 O003 1.4838(8) . ?
P001 N008 1.6518(10) . ?
P001 N00A 1.6449(11) . ?
P001 N00C 1.6510(10) . ?
P002 O005 1.4775(9) . ?
P002 N007 1.6467(11) . ?
P002 N009 1.6565(10) . ?
P002 N00G 1.6524(11) . ?
O004 C01D 1.2322(16) . ?
O006 H00B 0.8500 . ?
O006 H00D 0.8500 . ?
N007 H007 0.8600 . ?
N007 C00P 1.4015(15) . ?
N008 H008 0.8600 . ?
N008 C00N 1.3993(14) . ?
N009 H009 0.8600 . ?
N009 C00M 1.3985(14) . ?
N00A H00A 0.8601 . ?
N00A C00R 1.3984(14) . ?
N00B C00O 1.3360(15) . ?
N00B C00T 1.3521(15) . ?
N00C H00C 0.8600 . ?
N00C C00O 1.3969(14) . ?
N00D C00N 1.3364(15) . ?
N00D C016 1.3479(16) . ?
N00E C00Q 1.3382(15) . ?
N00E C010 1.3501(15) . ?
N00F C00M 1.3388(15) . ?
N00F C00Z 1.3458(15) . ?
N00G H00G 0.8600 . ?
N00G C00Q 1.3931(14) . ?
N00H C00P 1.3361(16) . ?
N00H C00Y 1.3474(17) . ?
O00I C01G 1.2331(19) . ?
N00J C01G 1.3328(18) . ?
N00J C01I 1.4528(17) . ?
N00J C01J 1.4540(19) . ?
N00K C01D 1.3324(17) . ?
N00K C01K 1.4557(17) . ?
N00K C01L 1.4543(18) . ?
N00L C00R 1.3380(16) . ?
N00L C01F 1.3445(17) . ?
C00M C01E 1.4043(16) . ?
C00N C00S 1.4014(16) . ?
C00O C013 1.4043(16) . ?
C00P C00X 1.4021(16) . ?
C00Q C00V 1.4105(16) . ?
C00R C00W 1.3995(16) . ?
C00S H00S 0.9300 . ?
C00S C012 1.3838(17) . ?
C00T H00T 0.9300 . ?
C00T C015 1.3784(18) . ?
C00U H00U 0.9300 . ?
C00U C013 1.3801(17) . ?
C00U C015 1.3965(19) . ?
C00V H00V 0.9300 . ?
C00V C01A 1.3819(18) . ?
C00W H00W 0.9300 . ?
C00W C011 1.3884(17) . ?
C00X H00X 0.9300 . ?
C00X C017 1.3846(17) . ?
C00Y H00Y 0.9300 . ?
C00Y C014 1.3843(19) . ?
C00Z H00Z 0.9300 . ?
C00Z C019 1.3845(18) . ?
C010 H010 0.9300 . ?
C010 C018 1.3840(18) . ?
C011 H011 0.9300 . ?
C011 C01B 1.385(2) . ?
C012 H012 0.9300 . ?
C012 C01C 1.3913(19) . ?
C013 H013 0.9300 . ?
C014 H014 0.9300 . ?
C014 C017 1.390(2) . ?
C015 H015 0.9300 . ?
C016 H016 0.9300 . ?
C016 C01C 1.379(2) . ?
C017 H017 0.9300 . ?
C018 H018 0.9300 . ?
C018 C01A 1.3961(19) . ?
C019 H019 0.9300 . ?
C019 C01H 1.3935(19) . ?
C01A H01A 0.9300 . ?
C01B H01B 0.9300 . ?
C01B C01F 1.381(2) . ?
C01C H01C 0.9300 . ?
C01D H01D 0.9300 . ?
C01E H01E 0.9300 . ?
C01E C01H 1.3838(18) . ?
C01F H01F 0.9300 . ?
C01G H01N 0.9300 . ?
C01H H01H 0.9300 . ?
C01I H01O 0.9600 . ?
C01I H01P 0.9600 . ?
C01I H01Q 0.9600 . ?
C01J H01R 0.9600 . ?
C01J H01S 0.9600 . ?
C01J H01T 0.9600 . ?
C01K H01G 0.9600 . ?
C01K H01I 0.9600 . ?
C01K H01J 0.9600 . ?
C01L H01K 0.9600 . ?
C01L H01L 0.9600 . ?
C01L H01M 0.9600 . ?
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
O003 P001 N008 115.36(5) . . ?
O003 P001 N00A 112.53(5) . . ?
O003 P001 N00C 108.76(5) . . ?
N00A P001 N008 103.59(5) . . ?
N00A P001 N00C 111.74(5) . . ?
N00C P001 N008 104.56(5) . . ?
O005 P002 N007 113.84(5) . . ?
O005 P002 N009 114.69(5) . . ?
O005 P002 N00G 108.39(6) . . ?
N007 P002 N009 103.13(6) . . ?
N007 P002 N00G 110.48(6) . . ?
N00G P002 N009 105.97(5) . . ?
H00B O006 H00D 104.5 . . ?
P002 N007 H007 108.5 . . ?
C00P N007 P002 127.03(9) . . ?
C00P N007 H007 108.5 . . ?
P001 N008 H008 116.4 . . ?
C00N N008 P001 127.29(8) . . ?
C00N N008 H008 116.4 . . ?
P002 N009 H009 116.8 . . ?
C00M N009 P002 126.45(8) . . ?
C00M N009 H009 116.8 . . ?
P001 N00A H00A 108.4 . . ?
C00R N00A P001 126.51(8) . . ?
C00R N00A H00A 108.4 . . ?
C00O N00B C00T 117.00(10) . . ?
P001 N00C H00C 115.4 . . ?
C00O N00C P001 129.15(8) . . ?
C00O N00C H00C 115.4 . . ?
C00N N00D C016 117.97(11) . . ?
C00Q N00E C010 117.15(10) . . ?
C00M N00F C00Z 118.39(10) . . ?
P002 N00G H00G 114.7 . . ?
C00Q N00G P002 130.50(8) . . ?
C00Q N00G H00G 114.7 . . ?
C00P N00H C00Y 117.19(11) . . ?
C01G N00J C01I 120.90(12) . . ?
C01G N00J C01J 122.01(12) . . ?
C01I N00J C01J 117.02(12) . . ?
C01D N00K C01K 121.40(12) . . ?
C01D N00K C01L 120.55(12) . . ?
C01L N00K C01K 117.92(12) . . ?
C00R N00L C01F 117.35(11) . . ?
N009 C00M C01E 122.89(10) . . ?
N00F C00M N009 114.64(10) . . ?
N00F C00M C01E 122.46(11) . . ?
N008 C00N C00S 122.71(10) . . ?
N00D C00N N008 114.64(10) . . ?
N00D C00N C00S 122.63(11) . . ?
N00B C00O N00C 118.65(10) . . ?
N00B C00O C013 123.13(11) . . ?
N00C C00O C013 118.22(10) . . ?
N007 C00P C00X 122.51(11) . . ?
N00H C00P N007 114.06(10) . . ?
N00H C00P C00X 123.42(11) . . ?
N00E C00Q N00G 118.78(10) . . ?
N00E C00Q C00V 122.91(11) . . ?
N00G C00Q C00V 118.31(10) . . ?
N00A C00R C00W 122.93(10) . . ?
N00L C00R N00A 114.22(10) . . ?
N00L C00R C00W 122.85(11) . . ?
C00N C00S H00S 121.0 . . ?
C012 C00S C00N 117.98(11) . . ?
C012 C00S H00S 121.0 . . ?
N00B C00T H00T 117.9 . . ?
N00B C00T C015 124.11(11) . . ?
C015 C00T H00T 117.9 . . ?
C013 C00U H00U 120.4 . . ?
C013 C00U C015 119.26(11) . . ?
C015 C00U H00U 120.4 . . ?
C00Q C00V H00V 120.8 . . ?
C01A C00V C00Q 118.45(11) . . ?
C01A C00V H00V 120.8 . . ?
C00R C00W H00W 121.0 . . ?
C011 C00W C00R 117.97(12) . . ?
C011 C00W H00W 121.0 . . ?
C00P C00X H00X 121.1 . . ?
C017 C00X C00P 117.88(12) . . ?
C017 C00X H00X 121.1 . . ?
N00H C00Y H00Y 118.1 . . ?
N00H C00Y C014 123.87(13) . . ?
C014 C00Y H00Y 118.1 . . ?
N00F C00Z H00Z 118.4 . . ?
N00F C00Z C019 123.28(11) . . ?
C019 C00Z H00Z 118.4 . . ?
N00E C010 H010 117.9 . . ?
N00E C010 C018 124.23(12) . . ?
C018 C010 H010 117.9 . . ?
C00W C011 H011 119.9 . . ?
C01B C011 C00W 120.14(12) . . ?
C01B C011 H011 119.9 . . ?
C00S C012 H012 120.0 . . ?
C00S C012 C01C 120.08(12) . . ?
C01C C012 H012 120.0 . . ?
C00O C013 H013 120.8 . . ?
C00U C013 C00O 118.46(11) . . ?
C00U C013 H013 120.8 . . ?
C00Y C014 H014 121.1 . . ?
C00Y C014 C017 117.88(12) . . ?
C017 C014 H014 121.1 . . ?
C00T C015 C00U 117.98(11) . . ?
C00T C015 H015 121.0 . . ?
C00U C015 H015 121.0 . . ?
N00D C016 H016 118.2 . . ?
N00D C016 C01C 123.67(12) . . ?
C01C C016 H016 118.2 . . ?
C00X C017 C014 119.73(12) . . ?
C00X C017 H017 120.1 . . ?
C014 C017 H017 120.1 . . ?
C010 C018 H018 121.1 . . ?
C010 C018 C01A 117.82(11) . . ?
C01A C018 H018 121.1 . . ?
C00Z C019 H019 121.1 . . ?
C00Z C019 C01H 117.77(11) . . ?
C01H C019 H019 121.1 . . ?
C00V C01A C018 119.41(12) . . ?
C00V C01A H01A 120.3 . . ?
C018 C01A H01A 120.3 . . ?
C011 C01B H01B 121.4 . . ?
C01F C01B C011 117.25(12) . . ?
C01F C01B H01B 121.4 . . ?
C012 C01C H01C 121.2 . . ?
C016 C01C C012 117.62(12) . . ?
C016 C01C H01C 121.2 . . ?
O004 C01D N00K 124.80(12) . . ?
O004 C01D H01D 117.6 . . ?
N00K C01D H01D 117.6 . . ?
C00M C01E H01E 121.0 . . ?
C01H C01E C00M 118.02(11) . . ?
C01H C01E H01E 121.0 . . ?
N00L C01F C01B 124.43(12) . . ?
N00L C01F H01F 117.8 . . ?
C01B C01F H01F 117.8 . . ?
O00I C01G N00J 125.05(14) . . ?
O00I C01G H01N 117.5 . . ?
N00J C01G H01N 117.5 . . ?
C019 C01H H01H 120.0 . . ?
C01E C01H C019 120.08(12) . . ?
C01E C01H H01H 120.0 . . ?
N00J C01I H01O 109.5 . . ?
N00J C01I H01P 109.5 . . ?
N00J C01I H01Q 109.5 . . ?
H01O C01I H01P 109.5 . . ?
H01O C01I H01Q 109.5 . . ?
H01P C01I H01Q 109.5 . . ?
N00J C01J H01R 109.5 . . ?
N00J C01J H01S 109.5 . . ?
N00J C01J H01T 109.5 . . ?
H01R C01J H01S 109.5 . . ?
H01R C01J H01T 109.5 . . ?
H01S C01J H01T 109.5 . . ?
N00K C01K H01G 109.5 . . ?
N00K C01K H01I 109.5 . . ?
N00K C01K H01J 109.5 . . ?
H01G C01K H01I 109.5 . . ?
H01G C01K H01J 109.5 . . ?
H01I C01K H01J 109.5 . . ?
N00K C01L H01K 109.5 . . ?
N00K C01L H01L 109.5 . . ?
N00K C01L H01M 109.5 . . ?
H01K C01L H01L 109.5 . . ?
H01K C01L H01M 109.5 . . ?
H01L C01L H01M 109.5 . . ?
_iucr_refine_instructions_details
;
TITL ms1k_c3_a.res in P2(1)/n
ms1k_c3.res
created by SHELXL-2018/1 at 14:40:08 on 24-Jul-2019
REM Old TITL ms1k_c3_a.res in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.104, Rweak 0.005, Alpha 0.031, Orientation as input
REM Formula found by SHELXT: C37 N13 O5 P2
CELL 0.7 10.625 18.707 20.479 90 98.249 90
ZERR 29 0.0021 0.0037 0.0041 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O P
DISP C 0.0033 0.0016 11.1819
DISP H -0 0 0.6234
DISP N 0.0063 0.0031 18.9823
DISP O 0.0112 0.0059 31.3712
DISP P 0.1018 0.0938 394.0833
UNIT 29 29 29 29 29
L.S. 10
PLAN 20
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.058000 2.004300
EXTI 0.076518
FVAR 0.73407
P001 5 0.456556 0.881619 0.477042 11.00000 0.01464 0.01026 =
0.01504 -0.00020 0.00242 0.00044
P002 5 0.753529 0.656536 0.451075 11.00000 0.01485 0.01393 =
0.01749 -0.00282 0.00056 0.00199
O003 4 0.388880 0.932380 0.515502 11.00000 0.01859 0.01306 =
0.01988 -0.00167 0.00532 0.00097
O004 4 0.979193 0.701011 0.331413 11.00000 0.02519 0.03432 =
0.02915 -0.01284 0.00879 -0.00514
O005 4 0.786753 0.592721 0.414610 11.00000 0.02213 0.01681 =
0.02408 -0.00635 0.00096 0.00345
AFIX 6
O006 4 0.668697 0.504992 0.314597 11.00000 0.04051 0.02359 =
0.02961 -0.00261 -0.00740 0.00000
H00B 2 0.700162 0.531012 0.346886 11.00000 -1.50000
H00D 2 0.648443 0.534262 0.283096 11.00000 -1.50000
AFIX 0
N007 3 0.752124 0.642320 0.530320 11.00000 0.01723 0.01526 =
0.01876 -0.00047 0.00094 0.00412
AFIX 3
H007 2 0.732374 0.681630 0.548120 11.00000 -1.20000
AFIX 0
N008 3 0.521528 0.812066 0.518706 11.00000 0.01392 0.01332 =
0.01859 0.00171 0.00214 0.00083
AFIX 43
H008 2 0.602957 0.808665 0.522368 11.00000 -1.20000
AFIX 0
N009 3 0.609822 0.689215 0.425973 11.00000 0.01570 0.01214 =
0.02062 0.00034 0.00036 0.00033
AFIX 43
H009 2 0.605404 0.733665 0.415169 11.00000 -1.20000
AFIX 0
N00A 3 0.361949 0.845247 0.415337 11.00000 0.01686 0.01193 =
0.01746 -0.00074 0.00033 0.00174
AFIX 3
H00A 2 0.405669 0.815587 0.395657 11.00000 -1.20000
AFIX 0
N00B 3 0.633968 0.837841 0.377027 11.00000 0.01954 0.01527 =
0.01818 -0.00103 0.00384 0.00034
N00C 3 0.577300 0.923543 0.451544 11.00000 0.01854 0.01138 =
0.01879 -0.00178 0.00545 -0.00166
AFIX 43
H00C 2 0.598113 0.963571 0.470766 11.00000 -1.20000
AFIX 0
N00D 3 0.534900 0.706518 0.577171 11.00000 0.02190 0.01636 =
0.01727 0.00209 0.00432 0.00330
N00E 3 0.807322 0.806190 0.517574 11.00000 0.01755 0.01846 =
0.01932 -0.00311 0.00160 0.00096
N00F 3 0.391048 0.691767 0.403646 11.00000 0.01671 0.01558 =
0.01819 -0.00092 0.00040 0.00091
N00G 3 0.854456 0.721146 0.440104 11.00000 0.01673 0.01828 =
0.01875 -0.00440 0.00442 -0.00037
AFIX 43
H00G 2 0.894720 0.715194 0.406955 11.00000 -1.20000
AFIX 0
N00H 3 0.819156 0.603561 0.636022 11.00000 0.02115 0.02155 =
0.02249 0.00211 0.00118 0.00213
O00I 4 0.601420 0.605427 0.215980 11.00000 0.04950 0.03082 =
0.03109 0.00085 0.00318 0.00562
N00J 3 0.491729 0.710089 0.214896 11.00000 0.03019 0.02680 =
0.02307 0.00202 0.00581 -0.00433
N00K 3 0.981820 0.641577 0.234801 11.00000 0.02882 0.02518 =
0.02110 -0.00349 0.00419 -0.00437
N00L 3 0.211188 0.838592 0.323094 11.00000 0.02121 0.02022 =
0.02616 -0.00228 -0.00330 0.00126
C00M 1 0.494978 0.651677 0.420611 11.00000 0.01679 0.01437 =
0.01560 -0.00123 0.00107 -0.00027
C00N 1 0.458922 0.758057 0.548709 11.00000 0.01908 0.01362 =
0.01415 -0.00043 0.00382 0.00065
C00O 1 0.650431 0.903191 0.403165 11.00000 0.01618 0.01455 =
0.01536 0.00165 0.00202 0.00153
C00P 1 0.845774 0.607698 0.574320 11.00000 0.01643 0.01315 =
0.02179 -0.00001 -0.00113 -0.00024
C00Q 1 0.884934 0.783692 0.475817 11.00000 0.01563 0.01628 =
0.01785 -0.00088 -0.00024 0.00080
C00R 1 0.278262 0.881365 0.367536 11.00000 0.01502 0.01598 =
0.01718 0.00085 0.00341 0.00198
C00S 1 0.326792 0.757239 0.547788 11.00000 0.01906 0.01937 =
0.02273 0.00148 0.00598 0.00195
AFIX 43
H00S 2 0.276265 0.794599 0.529043 11.00000 -1.20000
AFIX 0
C00T 1 0.703514 0.820803 0.328898 11.00000 0.02340 0.01950 =
0.01833 -0.00219 0.00383 0.00181
AFIX 43
H00T 2 0.692201 0.775715 0.309830 11.00000 -1.20000
AFIX 0
C00U 1 0.808927 0.933284 0.335782 11.00000 0.02433 0.02302 =
0.02506 0.00511 0.00912 -0.00152
AFIX 43
H00U 2 0.868070 0.964802 0.322544 11.00000 -1.20000
AFIX 0
C00V 1 0.996112 0.820845 0.465836 11.00000 0.01758 0.02189 =
0.02351 -0.00103 0.00310 -0.00061
AFIX 43
H00V 2 1.047317 0.804176 0.435895 11.00000 -1.20000
AFIX 0
C00W 1 0.265712 0.955841 0.366233 11.00000 0.03063 0.01617 =
0.02111 -0.00022 -0.00174 0.00327
AFIX 43
H00W 2 0.313382 0.984276 0.397862 11.00000 -1.20000
AFIX 0
C00X 1 0.956529 0.579334 0.554599 11.00000 0.01886 0.01913 =
0.02452 -0.00230 0.00049 0.00195
AFIX 43
H00X 2 0.970925 0.582169 0.510939 11.00000 -1.20000
AFIX 0
C00Y 1 0.905844 0.571530 0.681095 11.00000 0.02749 0.02646 =
0.02356 0.00444 -0.00082 0.00188
AFIX 43
H00Y 2 0.888360 0.568155 0.724203 11.00000 -1.20000
AFIX 0
C00Z 1 0.276650 0.659557 0.396693 11.00000 0.01662 0.02053 =
0.02540 -0.00296 0.00091 -0.00018
AFIX 43
H00Z 2 0.204477 0.687434 0.384955 11.00000 -1.20000
AFIX 0
C010 1 0.841159 0.866219 0.552301 11.00000 0.02232 0.02030 =
0.02135 -0.00471 0.00182 0.00158
AFIX 43
H010 2 0.788691 0.881887 0.582036 11.00000 -1.20000
AFIX 0
C011 1 0.179926 0.985977 0.316281 11.00000 0.03416 0.02039 =
0.02333 0.00321 0.00185 0.00887
AFIX 43
H011 2 0.169093 1.035301 0.314311 11.00000 -1.20000
AFIX 0
C012 1 0.273786 0.699152 0.575618 11.00000 0.02414 0.02468 =
0.02831 -0.00066 0.01170 -0.00324
AFIX 43
H012 2 0.186041 0.696089 0.574055 11.00000 -1.20000
AFIX 0
C013 1 0.738756 0.952412 0.384763 11.00000 0.02071 0.01508 =
0.02169 0.00230 0.00422 -0.00023
AFIX 43
H013 2 0.749710 0.996868 0.405110 11.00000 -1.20000
AFIX 0
C014 1 1.019398 0.543349 0.667026 11.00000 0.02396 0.02470 =
0.03022 0.00386 -0.00597 0.00380
AFIX 43
H014 2 1.077518 0.522656 0.699890 11.00000 -1.20000
AFIX 0
C015 1 0.790131 0.866072 0.306320 11.00000 0.02600 0.02735 =
0.01987 0.00055 0.00920 0.00223
AFIX 43
H015 2 0.834701 0.852274 0.272493 11.00000 -1.20000
AFIX 0
C016 1 0.480779 0.651584 0.605418 11.00000 0.03313 0.01665 =
0.02148 0.00425 0.00792 0.00384
AFIX 43
H016 2 0.533501 0.615906 0.625692 11.00000 -1.20000
AFIX 0
C017 1 1.043787 0.546968 0.602200 11.00000 0.01806 0.02117 =
0.03365 -0.00167 -0.00217 0.00422
AFIX 43
H017 2 1.118403 0.527728 0.590856 11.00000 -1.20000
AFIX 0
C018 1 0.948885 0.905947 0.546507 11.00000 0.02544 0.01975 =
0.02706 -0.00605 -0.00148 -0.00251
AFIX 43
H018 2 0.968478 0.946863 0.571716 11.00000 -1.20000
AFIX 0
C019 1 0.261032 0.586994 0.406141 11.00000 0.02029 0.02220 =
0.03620 -0.00342 0.00282 -0.00602
AFIX 43
H019 2 0.180540 0.566411 0.400969 11.00000 -1.20000
AFIX 0
C01A 1 1.027176 0.882587 0.501581 11.00000 0.02023 0.02141 =
0.03040 -0.00118 0.00102 -0.00441
AFIX 43
H01A 2 1.099597 0.908352 0.495761 11.00000 -1.20000
AFIX 0
C01B 1 0.110433 0.942736 0.269369 11.00000 0.02418 0.03229 =
0.02138 0.00179 -0.00110 0.01083
AFIX 43
H01B 2 0.053183 0.961978 0.235288 11.00000 -1.20000
AFIX 0
C01C 1 0.351607 0.645326 0.605936 11.00000 0.03543 0.01964 =
0.02822 0.00388 0.01377 -0.00324
AFIX 43
H01C 2 0.317724 0.606517 0.625838 11.00000 -1.20000
AFIX 0
C01D 1 0.931441 0.658919 0.288608 11.00000 0.02219 0.02784 =
0.02565 -0.00392 0.00555 -0.00376
AFIX 43
H01D 2 0.854596 0.637697 0.294274 11.00000 -1.20000
AFIX 0
C01E 1 0.488709 0.577672 0.431190 11.00000 0.02112 0.01476 =
0.03051 0.00128 0.00112 0.00080
AFIX 43
H01E 2 0.562185 0.550859 0.442910 11.00000 -1.20000
AFIX 0
C01F 1 0.129672 0.869880 0.275297 11.00000 0.02487 0.02978 =
0.02785 -0.00466 -0.00701 0.00336
AFIX 43
H01F 2 0.083085 0.840465 0.244115 11.00000 -1.20000
AFIX 0
C01G 1 0.522822 0.644510 0.237011 11.00000 0.03421 0.02795 =
0.02320 0.00027 0.00048 -0.00592
AFIX 43
H01N 2 0.482092 0.626860 0.270924 11.00000 -1.20000
AFIX 0
C01H 1 0.369953 0.545833 0.423658 11.00000 0.02734 0.01496 =
0.03927 0.00052 0.00359 -0.00381
AFIX 43
H01H 2 0.362824 0.496906 0.430294 11.00000 -1.20000
AFIX 0
C01I 1 0.553821 0.742428 0.163450 11.00000 0.03818 0.02758 =
0.02621 0.00172 0.00997 -0.00416
AFIX 137
H01O 2 0.616246 0.710022 0.150955 11.00000 -1.50000
H01P 2 0.594622 0.786029 0.179613 11.00000 -1.50000
H01Q 2 0.491623 0.752602 0.125786 11.00000 -1.50000
AFIX 0
C01J 1 0.399833 0.753740 0.243047 11.00000 0.02894 0.03598 =
0.03062 0.00434 0.00807 0.00013
AFIX 137
H01R 2 0.331909 0.766831 0.209040 11.00000 -1.50000
H01S 2 0.440822 0.796142 0.262044 11.00000 -1.50000
H01T 2 0.366093 0.727069 0.276643 11.00000 -1.50000
AFIX 0
C01K 1 0.920905 0.589850 0.187354 11.00000 0.04818 0.03801 =
0.02435 -0.01073 0.00522 -0.01053
AFIX 137
H01G 2 0.973302 0.547989 0.187868 11.00000 -1.50000
H01I 2 0.909759 0.610535 0.144008 11.00000 -1.50000
H01J 2 0.839480 0.576912 0.198897 11.00000 -1.50000
AFIX 0
C01L 1 1.104329 0.670431 0.224135 11.00000 0.03230 0.03767 =
0.02790 -0.00264 0.01189 -0.00449
AFIX 137
H01K 2 1.130199 0.706747 0.256401 11.00000 -1.50000
H01L 2 1.097245 0.690785 0.180729 11.00000 -1.50000
H01M 2 1.166412 0.632809 0.228234 11.00000 -1.50000
AFIX 0
HKLF 4
REM ms1k_c3_a.res in P2(1)/n
REM R1 = 0.0399 for 9586 Fo > 4sig(Fo) and 0.0402 for all 9811 data
REM 522 parameters refined using 0 restraints
END
WGHT 0.0580 2.0044
REM Highest difference peak 0.630, deepest hole -0.768, 1-sigma level 0.084
Q1 1 0.6835 0.6595 0.5482 11.00000 0.05 0.63
Q2 1 0.3639 0.8010 0.4098 11.00000 0.05 0.59
Q3 1 0.3950 0.7608 0.5531 11.00000 0.05 0.31
Q4 1 0.2733 0.9216 0.3661 11.00000 0.05 0.30
Q5 1 0.7581 0.6521 0.4990 11.00000 0.05 0.29
Q6 1 0.2334 0.9744 0.3385 11.00000 0.05 0.28
Q7 1 0.4011 0.8622 0.4391 11.00000 0.05 0.27
Q8 1 0.3286 0.8607 0.3973 11.00000 0.05 0.26
Q9 1 0.9672 0.5558 0.6732 11.00000 0.05 0.26
Q10 1 0.1464 0.9643 0.2906 11.00000 0.05 0.25
Q11 1 0.6568 0.8363 0.3510 11.00000 0.05 0.25
Q12 1 0.8017 0.6206 0.5504 11.00000 0.05 0.24
Q13 1 0.9068 0.5920 0.5644 11.00000 0.05 0.24
Q14 1 0.6575 0.6777 0.4421 11.00000 0.05 0.24
Q15 1 0.9420 0.8033 0.4719 11.00000 0.05 0.24
Q16 1 0.7239 0.5219 0.6873 11.00000 0.05 0.24
Q17 1 0.9902 0.5609 0.5800 11.00000 0.05 0.24
Q18 1 0.9056 0.9828 0.3399 11.00000 0.05 0.23
Q19 1 0.6291 0.5748 0.2433 11.00000 0.05 0.23
Q20 1 0.8577 0.5806 0.6552 11.00000 0.05 0.23
REM The information below was added by Olex2.
REM
REM R1 = 0.0399 for 9586 Fo > 4sig(Fo) and 0.0402 for all 58515 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.63, deepest hole -0.77
REM Mean Shift 0, Max Shift 0.002.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0402
REM R1_gt = 0.0399
REM wR_ref = 0.1069
REM GOOF = 1.060
REM Shift_max = 0.002
REM Shift_mean = 0
REM Reflections_all = 58515
REM Reflections_gt = 9586
REM Parameters = n/a
REM Hole = -0.77
REM Peak = 0.63
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'