data_4
_audit_creation_date 2013-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number 2013-4
_publ_contact_author_address ?
_publ_contact_author_email ?
_publ_contact_author_name ''
_publ_contact_author_phone ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C80 H70 N4 P2 S2 Zn'
_chemical_formula_sum 'C80 H70 N4 P2 S2 Zn'
_chemical_formula_weight 1278.83
_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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Zn' 'Zn' -1.5491 0.6778
'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 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 28.4395(15)
_cell_length_b 18.7648(11)
_cell_length_c 16.3621(9)
_cell_angle_alpha 90
_cell_angle_beta 123.051(3)
_cell_angle_gamma 90
_cell_volume 7318.9(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9871
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 64.985
_cell_measurement_theta_min 3.586
_shelx_estimated_absorpt_T_max 0.932
_shelx_estimated_absorpt_T_min 0.547
_exptl_absorpt_coefficient_mu 1.745
_exptl_absorpt_correction_T_max 0.7526
_exptl_absorpt_correction_T_min 0.6294
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.161
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2680
_exptl_crystal_size_max 0.393
_exptl_crystal_size_mid 0.142
_exptl_crystal_size_min 0.041
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0398
_diffrn_reflns_av_unetI/netI 0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_h_min -33
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 56300
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 65.04
_diffrn_reflns_theta_min 2.99
_diffrn_ambient_temperature 100.05
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'Quazar optics'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source microsource
_diffrn_standards_number .
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5371
_reflns_number_total 6214
_reflns_special_details
;
Data were apparently pre-merged, so _diffrn_reflns_number
etc. will have to be added later.
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 'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max 0.829
_refine_diff_density_min -0.614
_refine_diff_density_rms 0.077
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.087
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 406
_refine_ls_number_reflns 6214
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0608
_refine_ls_R_factor_gt 0.0541
_refine_ls_restrained_S_all 1.087
_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^)+(0.1006P)^2^+12.2253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1604
_refine_ls_wR_factor_ref 0.1661
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C7(H7), C8(H8), C13(H13), C15(H15), C21(H21), C22(H22),
C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
C37(H37), C38(H38), C39(H39), C40(H40)
2.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_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
Zn1 Zn 0.2500 0.7500 0.0000 0.03484(19) Uani 1 2 d S . P . .
S1 S 0.62745(3) 0.55399(5) 0.14103(6) 0.0456(2) Uani 1 1 d . . . . .
P1 P 0.77194(3) 0.61736(4) 0.42976(5) 0.0335(2) Uani 1 1 d . . . . .
N1 N 0.16828(8) 0.75297(11) -0.11265(15) 0.0226(4) Uani 1 1 d . . . . .
N2 N 0.27020(8) 0.69452(12) -0.08526(14) 0.0247(4) Uani 1 1 d . . . . .
C1 C 0.12557(10) 0.78859(14) -0.11519(18) 0.0276(6) Uani 1 1 d . . . . .
C2 C 0.07531(11) 0.78158(19) -0.2100(2) 0.0417(7) Uani 1 1 d . . . . .
H2 H 0.0400 0.8024 -0.2313 0.050 Uiso 1 1 calc R U . . .
C3 C 0.08732(11) 0.73981(18) -0.2639(2) 0.0385(7) Uani 1 1 d . . . . .
H3 H 0.0619 0.7250 -0.3294 0.046 Uiso 1 1 calc R U . . .
C4 C 0.14607(10) 0.72217(14) -0.20289(17) 0.0249(5) Uani 1 1 d . . . . .
C5 C 0.17521(11) 0.68200(14) -0.23331(17) 0.0275(5) Uani 1 1 d . . . . .
C6 C 0.23309(11) 0.66992(14) -0.17853(18) 0.0278(5) Uani 1 1 d . . . . .
C7 C 0.26325(12) 0.62805(16) -0.2096(2) 0.0341(6) Uani 1 1 d . . . . .
H7 H 0.2477 0.6056 -0.2712 0.041 Uiso 1 1 calc R U . . .
C8 C 0.31748(11) 0.62676(15) -0.1351(2) 0.0332(6) Uani 1 1 d . . . . .
H8 H 0.3473 0.6032 -0.1344 0.040 Uiso 1 1 calc R U . . .
C9 C 0.32202(10) 0.66752(14) -0.05660(18) 0.0269(5) Uani 1 1 d . . . . .
C10 C 0.37031(10) 0.67422(14) 0.03708(19) 0.0284(6) Uani 1 1 d . . . . .
C11 C 0.14009(11) 0.64915(16) -0.33387(18) 0.0320(6) Uani 1 1 d . . . . .
C12 C 0.13063(13) 0.68719(18) -0.4151(2) 0.0404(7) Uani 1 1 d . . . . .
C13 C 0.09398(13) 0.6576(2) -0.5078(2) 0.0479(8) Uani 1 1 d . . . . .
H13 H 0.0858 0.6839 -0.5638 0.057 Uiso 1 1 calc R U . . .
C14 C 0.06940(12) 0.59177(19) -0.5204(2) 0.0452(8) Uani 1 1 d . . . . .
C15 C 0.08046(12) 0.55463(18) -0.4396(2) 0.0408(7) Uani 1 1 d . . . . .
H15 H 0.0640 0.5090 -0.4477 0.049 Uiso 1 1 calc R U . . .
C16 C 0.11524(11) 0.58219(17) -0.3456(2) 0.0356(6) Uani 1 1 d . . . . .
C17 C 0.15722(18) 0.7576(2) -0.4041(3) 0.0572(10) Uani 1 1 d . . . . .
H17A H 0.1440 0.7915 -0.3755 0.086 Uiso 1 1 calc R U . . .
H17B H 0.1472 0.7749 -0.4682 0.086 Uiso 1 1 calc R U . . .
H17C H 0.1981 0.7528 -0.3614 0.086 Uiso 1 1 calc R U . . .
C18 C 0.03088(15) 0.5606(2) -0.6222(2) 0.0616(10) Uani 1 1 d . . . . .
H18A H 0.0532 0.5461 -0.6484 0.092 Uiso 1 1 calc R U . . .
H18B H 0.0034 0.5967 -0.6649 0.092 Uiso 1 1 calc R U . . .
H18C H 0.0112 0.5191 -0.6186 0.092 Uiso 1 1 calc R U . . .
C19 C 0.12394(15) 0.54051(19) -0.2604(2) 0.0502(8) Uani 1 1 d . . . . .
H19A H 0.1633 0.5439 -0.2064 0.075 Uiso 1 1 calc R U . . .
H19B H 0.1142 0.4905 -0.2792 0.075 Uiso 1 1 calc R U . . .
H19C H 0.1000 0.5599 -0.2398 0.075 Uiso 1 1 calc R U . . .
C20 C 0.42212(11) 0.63443(16) 0.05896(19) 0.0329(6) Uani 1 1 d . . . . .
C21 C 0.45819(12) 0.66090(17) 0.0371(3) 0.0489(8) Uani 1 1 d . . . . .
H21 H 0.4505 0.7053 0.0042 0.059 Uiso 1 1 calc R U . . .
C22 C 0.50724(13) 0.62268(18) 0.0629(3) 0.0550(10) Uani 1 1 d . . . . .
H22 H 0.5328 0.6423 0.0488 0.066 Uiso 1 1 calc R U . . .
C23 C 0.51840(11) 0.55792(17) 0.1078(2) 0.0392(7) Uani 1 1 d . . . . .
C24 C 0.4821(2) 0.5317(3) 0.1264(4) 0.098(2) Uani 1 1 d . . . . .
H24 H 0.4889 0.4861 0.1561 0.117 Uiso 1 1 calc R U . . .
C25 C 0.4342(2) 0.5692(3) 0.1035(4) 0.100(2) Uani 1 1 d . . . . .
H25 H 0.4093 0.5492 0.1191 0.120 Uiso 1 1 calc R U . . .
C26 C 0.56854(12) 0.51150(19) 0.1308(3) 0.0501(9) Uani 1 1 d . . . . .
H26A H 0.5548 0.4747 0.0793 0.060 Uiso 1 1 calc R U . . .
H26B H 0.5818 0.4863 0.1929 0.060 Uiso 1 1 calc R U . . .
C27 C 0.66662(14) 0.58008(18) 0.2676(2) 0.0447(7) Uani 1 1 d . . . . .
H27A H 0.6492 0.6225 0.2766 0.054 Uiso 1 1 calc R U . . .
H27B H 0.6667 0.5409 0.3082 0.054 Uiso 1 1 calc R U . . .
C28 C 0.72679(12) 0.59723(18) 0.2985(2) 0.0400(7) Uani 1 1 d . . . . .
H28A H 0.7264 0.6387 0.2607 0.048 Uiso 1 1 calc R U . . .
H28B H 0.7425 0.5561 0.2833 0.048 Uiso 1 1 calc R U . . .
C29 C 0.77212(12) 0.53096(16) 0.4819(2) 0.0365(6) Uani 1 1 d . . . . .
C30 C 0.80380(14) 0.47230(18) 0.4887(3) 0.0479(8) Uani 1 1 d . . . . .
H30 H 0.8283 0.4756 0.4663 0.058 Uiso 1 1 calc R U . . .
C31 C 0.79977(19) 0.4089(2) 0.5280(4) 0.0700(12) Uani 1 1 d . . . . .
H31 H 0.8218 0.3691 0.5328 0.084 Uiso 1 1 calc R U . . .
C32 C 0.76418(19) 0.4028(2) 0.5604(4) 0.0694(12) Uani 1 1 d . . . . .
H32 H 0.7618 0.3593 0.5875 0.083 Uiso 1 1 calc R U . . .
C33 C 0.73235(17) 0.4603(2) 0.5530(3) 0.0606(10) Uani 1 1 d . . . . .
H33 H 0.7073 0.4564 0.5743 0.073 Uiso 1 1 calc R U . . .
C34 C 0.73638(13) 0.52338(18) 0.5151(3) 0.0459(8) Uani 1 1 d . . . . .
H34 H 0.7144 0.5629 0.5113 0.055 Uiso 1 1 calc R U . . .
C35 C 0.84199(12) 0.62319(15) 0.4500(2) 0.0361(6) Uani 1 1 d . . . . .
C36 C 0.85110(14) 0.63389(19) 0.3754(2) 0.0470(8) Uani 1 1 d . . . . .
H36 H 0.8202 0.6337 0.3094 0.056 Uiso 1 1 calc R U . . .
C37 C 0.90480(15) 0.6448(2) 0.3969(3) 0.0569(9) Uani 1 1 d . . . . .
H37 H 0.9106 0.6520 0.3455 0.068 Uiso 1 1 calc R U . . .
C38 C 0.94993(14) 0.64537(18) 0.4921(3) 0.0522(9) Uani 1 1 d . . . . .
H38 H 0.9867 0.6528 0.5064 0.063 Uiso 1 1 calc R U . . .
C39 C 0.94170(13) 0.63518(17) 0.5666(3) 0.0455(8) Uani 1 1 d . . . . .
H39 H 0.9728 0.6354 0.6324 0.055 Uiso 1 1 calc R U . . .
C40 C 0.88767(12) 0.62456(17) 0.5454(2) 0.0400(7) Uani 1 1 d . . . . .
H40 H 0.8821 0.6182 0.5972 0.048 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0142(3) 0.0624(4) 0.0224(3) -0.0122(2) 0.0064(2) 0.0033(2)
S1 0.0269(4) 0.0641(5) 0.0389(4) -0.0162(3) 0.0135(3) 0.0071(3)
P1 0.0234(4) 0.0414(4) 0.0332(4) -0.0027(3) 0.0138(3) 0.0001(3)
N1 0.0150(10) 0.0326(11) 0.0173(10) 0.0000(8) 0.0068(9) 0.0026(8)
N2 0.0160(10) 0.0360(11) 0.0184(10) -0.0021(8) 0.0070(8) 0.0046(8)
C1 0.0158(12) 0.0406(15) 0.0225(13) 0.0025(11) 0.0080(10) 0.0048(10)
C2 0.0165(13) 0.075(2) 0.0259(14) -0.0019(14) 0.0065(12) 0.0147(13)
C3 0.0154(13) 0.069(2) 0.0197(13) -0.0045(13) 0.0025(11) 0.0050(12)
C4 0.0157(12) 0.0369(13) 0.0170(11) -0.0002(10) 0.0056(10) 0.0002(10)
C5 0.0218(12) 0.0366(14) 0.0174(12) -0.0027(10) 0.0064(10) -0.0014(11)
C6 0.0233(13) 0.0366(14) 0.0203(12) -0.0022(10) 0.0098(11) 0.0033(11)
C7 0.0297(14) 0.0459(16) 0.0249(13) -0.0100(12) 0.0136(12) 0.0016(12)
C8 0.0271(14) 0.0434(15) 0.0303(14) -0.0033(12) 0.0164(12) 0.0078(12)
C9 0.0209(12) 0.0355(14) 0.0238(12) 0.0006(10) 0.0120(11) 0.0058(10)
C10 0.0195(12) 0.0389(15) 0.0266(13) 0.0036(11) 0.0124(11) 0.0081(11)
C11 0.0220(13) 0.0487(16) 0.0193(12) -0.0069(11) 0.0073(11) 0.0053(12)
C12 0.0375(16) 0.0539(18) 0.0237(14) -0.0039(13) 0.0126(13) 0.0072(14)
C13 0.0428(17) 0.071(2) 0.0235(14) -0.0007(14) 0.0137(14) 0.0128(16)
C14 0.0294(15) 0.065(2) 0.0273(15) -0.0161(14) 0.0068(12) 0.0080(15)
C15 0.0264(14) 0.0555(19) 0.0301(15) -0.0158(13) 0.0086(12) 0.0002(13)
C16 0.0223(13) 0.0514(17) 0.0267(14) -0.0124(12) 0.0092(11) -0.0010(12)
C17 0.068(2) 0.065(2) 0.0300(17) 0.0042(15) 0.0213(17) -0.0036(18)
C18 0.049(2) 0.084(3) 0.0252(16) -0.0195(17) 0.0033(15) 0.0064(19)
C19 0.0504(19) 0.056(2) 0.0362(16) -0.0123(15) 0.0181(15) -0.0171(16)
C20 0.0191(13) 0.0493(16) 0.0249(13) -0.0013(12) 0.0084(11) 0.0107(12)
C21 0.0272(15) 0.0349(15) 0.084(3) -0.0084(16) 0.0303(17) 0.0001(13)
C22 0.0259(15) 0.0464(19) 0.093(3) -0.0175(18) 0.0329(18) -0.0068(14)
C23 0.0228(14) 0.0473(17) 0.0295(14) -0.0116(12) 0.0027(12) 0.0071(12)
C24 0.087(3) 0.112(4) 0.134(4) 0.084(4) 0.086(3) 0.072(3)
C25 0.087(3) 0.118(4) 0.146(5) 0.098(4) 0.096(4) 0.079(3)
C26 0.0257(15) 0.055(2) 0.0497(18) -0.0210(15) 0.0075(14) 0.0070(14)
C27 0.0442(18) 0.0503(18) 0.0407(17) -0.0122(14) 0.0239(15) -0.0024(14)
C28 0.0316(15) 0.0496(17) 0.0341(15) -0.0052(13) 0.0148(13) 0.0012(13)
C29 0.0278(14) 0.0434(16) 0.0373(15) -0.0053(12) 0.0172(13) -0.0028(12)
C30 0.0451(18) 0.0512(18) 0.063(2) 0.0066(16) 0.0393(17) 0.0070(15)
C31 0.077(3) 0.051(2) 0.113(4) 0.016(2) 0.072(3) 0.017(2)
C32 0.084(3) 0.053(2) 0.102(3) 0.017(2) 0.070(3) 0.004(2)
C33 0.066(2) 0.059(2) 0.087(3) -0.001(2) 0.061(2) -0.0037(18)
C34 0.0369(16) 0.0519(19) 0.057(2) -0.0054(15) 0.0312(16) -0.0010(14)
C35 0.0280(14) 0.0387(15) 0.0420(16) -0.0028(12) 0.0193(13) 0.0003(12)
C36 0.0387(17) 0.062(2) 0.0448(18) -0.0075(15) 0.0254(15) -0.0063(15)
C37 0.050(2) 0.071(2) 0.066(2) -0.0124(19) 0.042(2) -0.0075(18)
C38 0.0352(17) 0.0483(19) 0.080(3) -0.0119(17) 0.0360(19) -0.0041(14)
C39 0.0291(15) 0.0419(17) 0.056(2) -0.0058(14) 0.0174(15) 0.0011(13)
C40 0.0312(15) 0.0456(17) 0.0421(17) -0.0013(13) 0.0193(14) 0.0015(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.032(2) 7_565 ?
Zn1 N1 2.032(2) . ?
Zn1 N2 2.058(2) . ?
Zn1 N2 2.058(2) 7_565 ?
S1 C26 1.779(4) . ?
S1 C27 1.804(3) . ?
P1 C28 1.843(3) . ?
P1 C29 1.831(3) . ?
P1 C35 1.836(3) . ?
N1 C1 1.367(3) . ?
N1 C4 1.377(3) . ?
N2 C6 1.378(3) . ?
N2 C9 1.376(3) . ?
C1 C2 1.431(4) . ?
C1 C10 1.404(4) 7_565 ?
C2 H2 0.9500 . ?
C2 C3 1.355(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.442(4) . ?
C4 C5 1.397(4) . ?
C5 C6 1.398(4) . ?
C5 C11 1.514(3) . ?
C6 C7 1.445(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.347(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.438(4) . ?
C9 C10 1.398(4) . ?
C10 C1 1.404(4) 7_565 ?
C10 C20 1.510(3) . ?
C11 C12 1.400(4) . ?
C11 C16 1.403(4) . ?
C12 C13 1.404(4) . ?
C12 C17 1.483(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.378(5) . ?
C14 C15 1.372(5) . ?
C14 C18 1.524(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.396(4) . ?
C16 C19 1.497(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.352(4) . ?
C20 C25 1.369(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.413(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.365(5) . ?
C23 C24 1.319(5) . ?
C23 C26 1.532(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(5) . ?
C25 H25 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.531(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.388(4) . ?
C29 C34 1.397(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.387(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.379(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.371(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.369(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(4) . ?
C35 C40 1.383(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.383(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.376(5) . ?
C38 H38 0.9500 . ?
C38 C39 1.374(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.393(4) . ?
C40 H40 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N1 180.00(10) 7_565 . ?
N1 Zn1 N2 89.83(8) 7_565 . ?
N1 Zn1 N2 90.17(8) . . ?
N1 Zn1 N2 90.17(8) 7_565 7_565 ?
N1 Zn1 N2 89.83(8) . 7_565 ?
N2 Zn1 N2 180.0 . 7_565 ?
C26 S1 C27 100.93(16) . . ?
C29 P1 C28 100.64(14) . . ?
C29 P1 C35 103.99(13) . . ?
C35 P1 C28 102.72(14) . . ?
C1 N1 Zn1 126.77(17) . . ?
C1 N1 C4 107.0(2) . . ?
C4 N1 Zn1 126.15(16) . . ?
C6 N2 Zn1 126.29(16) . . ?
C9 N2 Zn1 126.74(16) . . ?
C9 N2 C6 106.6(2) . . ?
N1 C1 C2 109.5(2) . . ?
N1 C1 C10 125.7(2) . 7_565 ?
C10 C1 C2 124.8(2) 7_565 . ?
C1 C2 H2 126.2 . . ?
C3 C2 C1 107.5(2) . . ?
C3 C2 H2 126.2 . . ?
C2 C3 H3 126.6 . . ?
C2 C3 C4 106.9(2) . . ?
C4 C3 H3 126.6 . . ?
N1 C4 C3 109.1(2) . . ?
N1 C4 C5 126.5(2) . . ?
C5 C4 C3 124.5(2) . . ?
C4 C5 C6 125.4(2) . . ?
C4 C5 C11 116.0(2) . . ?
C6 C5 C11 118.6(2) . . ?
N2 C6 C5 125.3(2) . . ?
N2 C6 C7 109.2(2) . . ?
C5 C6 C7 125.4(2) . . ?
C6 C7 H7 126.4 . . ?
C8 C7 C6 107.3(2) . . ?
C8 C7 H7 126.4 . . ?
C7 C8 H8 126.3 . . ?
C7 C8 C9 107.5(2) . . ?
C9 C8 H8 126.3 . . ?
N2 C9 C8 109.5(2) . . ?
N2 C9 C10 124.7(2) . . ?
C10 C9 C8 125.6(2) . . ?
C1 C10 C20 116.3(2) 7_565 . ?
C9 C10 C1 125.9(2) . 7_565 ?
C9 C10 C20 117.6(2) . . ?
C12 C11 C5 119.7(3) . . ?
C12 C11 C16 120.3(3) . . ?
C16 C11 C5 119.9(2) . . ?
C11 C12 C13 118.0(3) . . ?
C11 C12 C17 121.2(3) . . ?
C13 C12 C17 120.8(3) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 C12 122.2(3) . . ?
C14 C13 H13 118.9 . . ?
C13 C14 C18 120.7(3) . . ?
C15 C14 C13 118.7(3) . . ?
C15 C14 C18 120.6(3) . . ?
C14 C15 H15 119.1 . . ?
C14 C15 C16 121.7(3) . . ?
C16 C15 H15 119.1 . . ?
C11 C16 C19 121.7(2) . . ?
C15 C16 C11 119.0(3) . . ?
C15 C16 C19 119.3(3) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C10 122.6(3) . . ?
C21 C20 C25 117.6(3) . . ?
C25 C20 C10 119.8(3) . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.1(3) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C26 123.4(3) . . ?
C24 C23 C22 118.4(3) . . ?
C24 C23 C26 118.1(3) . . ?
C23 C24 H24 119.2 . . ?
C23 C24 C25 121.5(4) . . ?
C25 C24 H24 119.2 . . ?
C20 C25 C24 121.3(4) . . ?
C20 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
S1 C26 H26A 107.8 . . ?
S1 C26 H26B 107.8 . . ?
C23 C26 S1 118.1(3) . . ?
C23 C26 H26A 107.8 . . ?
C23 C26 H26B 107.8 . . ?
H26A C26 H26B 107.1 . . ?
S1 C27 H27A 110.0 . . ?
S1 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
C28 C27 S1 108.4(2) . . ?
C28 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
P1 C28 H28A 109.3 . . ?
P1 C28 H28B 109.3 . . ?
C27 C28 P1 111.8(2) . . ?
C27 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 P1 125.2(2) . . ?
C30 C29 C34 117.8(3) . . ?
C34 C29 P1 117.0(2) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.9(3) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 120.4 . . ?
C33 C32 C31 119.2(4) . . ?
C33 C32 H32 120.4 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.4(3) . . ?
C34 C33 H33 119.8 . . ?
C29 C34 H34 119.3 . . ?
C33 C34 C29 121.5(3) . . ?
C33 C34 H34 119.3 . . ?
C36 C35 P1 123.5(2) . . ?
C40 C35 P1 117.6(2) . . ?
C40 C35 C36 118.5(3) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 C35 120.4(3) . . ?
C37 C36 H36 119.8 . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.5(3) . . ?
C38 C37 H37 119.8 . . ?
C37 C38 H38 120.0 . . ?
C39 C38 C37 119.9(3) . . ?
C39 C38 H38 120.0 . . ?
C38 C39 H39 120.1 . . ?
C38 C39 C40 119.8(3) . . ?
C40 C39 H39 120.1 . . ?
C35 C40 C39 120.9(3) . . ?
C35 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N1 C1 C2 175.8(2) . . . . ?
Zn1 N1 C1 C10 -4.9(4) . . . 7_565 ?
Zn1 N1 C4 C3 -176.73(19) . . . . ?
Zn1 N1 C4 C5 1.4(4) . . . . ?
Zn1 N2 C6 C5 3.7(4) . . . . ?
Zn1 N2 C6 C7 -174.74(18) . . . . ?
Zn1 N2 C9 C8 174.74(18) . . . . ?
Zn1 N2 C9 C10 -0.5(4) . . . . ?
S1 C27 C28 P1 -175.27(17) . . . . ?
P1 C29 C30 C31 -178.8(3) . . . . ?
P1 C29 C34 C33 178.3(3) . . . . ?
P1 C35 C36 C37 173.5(3) . . . . ?
P1 C35 C40 C39 -174.3(2) . . . . ?
N1 C1 C2 C3 1.8(4) . . . . ?
N1 C4 C5 C6 -4.2(4) . . . . ?
N1 C4 C5 C11 175.4(2) . . . . ?
N2 C6 C7 C8 1.0(3) . . . . ?
N2 C9 C10 C1 -2.6(4) . . . 7_565 ?
N2 C9 C10 C20 173.4(2) . . . . ?
C1 N1 C4 C3 0.4(3) . . . . ?
C1 N1 C4 C5 178.4(3) . . . . ?
C1 C2 C3 C4 -1.5(4) . . . . ?
C1 C10 C20 C21 -99.2(3) 7_565 . . . ?
C1 C10 C20 C25 80.2(5) 7_565 . . . ?
C2 C3 C4 N1 0.8(3) . . . . ?
C2 C3 C4 C5 -177.4(3) . . . . ?
C3 C4 C5 C6 173.6(3) . . . . ?
C3 C4 C5 C11 -6.8(4) . . . . ?
C4 N1 C1 C2 -1.3(3) . . . . ?
C4 N1 C1 C10 178.0(3) . . . 7_565 ?
C4 C5 C6 N2 1.4(4) . . . . ?
C4 C5 C6 C7 179.6(3) . . . . ?
C4 C5 C11 C12 90.1(3) . . . . ?
C4 C5 C11 C16 -87.1(3) . . . . ?
C5 C6 C7 C8 -177.4(3) . . . . ?
C5 C11 C12 C13 -174.6(3) . . . . ?
C5 C11 C12 C17 3.7(4) . . . . ?
C5 C11 C16 C15 176.4(2) . . . . ?
C5 C11 C16 C19 -2.0(4) . . . . ?
C6 N2 C9 C8 1.8(3) . . . . ?
C6 N2 C9 C10 -173.5(3) . . . . ?
C6 C5 C11 C12 -90.2(3) . . . . ?
C6 C5 C11 C16 92.5(3) . . . . ?
C6 C7 C8 C9 0.0(3) . . . . ?
C7 C8 C9 N2 -1.1(3) . . . . ?
C7 C8 C9 C10 174.1(3) . . . . ?
C8 C9 C10 C1 -177.1(3) . . . 7_565 ?
C8 C9 C10 C20 -1.1(4) . . . . ?
C9 N2 C6 C5 176.7(3) . . . . ?
C9 N2 C6 C7 -1.7(3) . . . . ?
C9 C10 C20 C21 84.3(4) . . . . ?
C9 C10 C20 C25 -96.3(4) . . . . ?
C10 C1 C2 C3 -177.5(3) 7_565 . . . ?
C10 C20 C21 C22 177.3(3) . . . . ?
C10 C20 C25 C24 -178.8(5) . . . . ?
C11 C5 C6 N2 -178.2(2) . . . . ?
C11 C5 C6 C7 0.0(4) . . . . ?
C11 C12 C13 C14 -2.8(5) . . . . ?
C12 C11 C16 C15 -0.8(4) . . . . ?
C12 C11 C16 C19 -179.2(3) . . . . ?
C12 C13 C14 C15 1.2(5) . . . . ?
C12 C13 C14 C18 -178.6(3) . . . . ?
C13 C14 C15 C16 0.8(4) . . . . ?
C14 C15 C16 C11 -0.9(4) . . . . ?
C14 C15 C16 C19 177.5(3) . . . . ?
C16 C11 C12 C13 2.6(4) . . . . ?
C16 C11 C12 C17 -179.0(3) . . . . ?
C17 C12 C13 C14 178.8(3) . . . . ?
C18 C14 C15 C16 -179.5(3) . . . . ?
C20 C21 C22 C23 1.7(5) . . . . ?
C21 C20 C25 C24 0.7(8) . . . . ?
C21 C22 C23 C24 0.2(6) . . . . ?
C21 C22 C23 C26 175.3(3) . . . . ?
C22 C23 C24 C25 -1.6(8) . . . . ?
C22 C23 C26 S1 23.3(4) . . . . ?
C23 C24 C25 C20 1.3(10) . . . . ?
C24 C23 C26 S1 -161.6(4) . . . . ?
C25 C20 C21 C22 -2.1(6) . . . . ?
C26 S1 C27 C28 163.0(2) . . . . ?
C26 C23 C24 C25 -177.0(5) . . . . ?
C27 S1 C26 C23 86.5(3) . . . . ?
C28 P1 C29 C30 78.0(3) . . . . ?
C28 P1 C29 C34 -100.3(3) . . . . ?
C28 P1 C35 C36 19.1(3) . . . . ?
C28 P1 C35 C40 -168.1(2) . . . . ?
C29 P1 C28 C27 65.2(3) . . . . ?
C29 P1 C35 C36 123.6(3) . . . . ?
C29 P1 C35 C40 -63.5(3) . . . . ?
C29 C30 C31 C32 0.4(7) . . . . ?
C30 C29 C34 C33 -0.2(5) . . . . ?
C30 C31 C32 C33 0.2(8) . . . . ?
C31 C32 C33 C34 -0.9(7) . . . . ?
C32 C33 C34 C29 0.8(6) . . . . ?
C34 C29 C30 C31 -0.4(5) . . . . ?
C35 P1 C28 C27 172.4(2) . . . . ?
C35 P1 C29 C30 -28.1(3) . . . . ?
C35 P1 C29 C34 153.6(2) . . . . ?
C35 C36 C37 C38 -0.1(6) . . . . ?
C36 C35 C40 C39 -1.1(5) . . . . ?
C36 C37 C38 C39 -0.2(6) . . . . ?
C37 C38 C39 C40 -0.2(5) . . . . ?
C38 C39 C40 C35 0.8(5) . . . . ?
C40 C35 C36 C37 0.7(5) . . . . ?
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement. As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.
Total solvent accessible volume / cell = 1441.7 Ang^3^ [19.7%]
Total electron count / cell = 278.4
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.776 0.250 -0.026 720.8 139.2 ?
2 -0.455 0.750 -0.205 720.8 139.2 ?
_shelx_res_file
;
TITL n3163 in C2/c
CELL 1.54178 28.4395 18.7648 16.3621 90 123.0512 90
ZERR 4 0.0015 0.0011 0.0009 0 0.0026 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N P S Zn
UNIT 320 280 16 8 8 4
L.S. 4
PLAN 20
SIZE 0.041 0.142 0.393
TEMP -173.1
REM Solution 1 R1 0.240, Alpha = 0.0479 in C2/c
REM Formula: C74 N10 S2 Zn3
BOND $h
fmap 2
acta
wpdb -2
MORE -1
CONF
REM R:/XRAYWORKING/Charlotte/n3163/n3163-mask.hkl
WGHT 0.100600 12.225301
FVAR 0.05492
ZN1 6 0.250000 0.750000 0.000000 10.50000 0.01419 0.06239 =
0.02238 -0.01215 0.00639 0.00332
S1 5 0.627452 0.553994 0.141034 11.00000 0.02694 0.06414 =
0.03892 -0.01622 0.01349 0.00715
P1 4 0.771940 0.617358 0.429756 11.00000 0.02344 0.04140 =
0.03321 -0.00265 0.01380 0.00005
N1 3 0.168276 0.752974 -0.112654 11.00000 0.01498 0.03261 =
0.01727 0.00000 0.00685 0.00263
N2 3 0.270199 0.694516 -0.085262 11.00000 0.01602 0.03600 =
0.01844 -0.00212 0.00704 0.00456
C1 1 0.125572 0.788594 -0.115186 11.00000 0.01583 0.04061 =
0.02254 0.00246 0.00795 0.00478
C2 1 0.075307 0.781578 -0.210013 11.00000 0.01654 0.07496 =
0.02586 -0.00192 0.00653 0.01468
AFIX 43
H2 2 0.039963 0.802401 -0.231300 11.00000 -1.20000
AFIX 0
C3 1 0.087324 0.739811 -0.263905 11.00000 0.01540 0.06946 =
0.01971 -0.00447 0.00255 0.00504
AFIX 43
H3 2 0.061896 0.724999 -0.329364 11.00000 -1.20000
AFIX 0
C4 1 0.146075 0.722166 -0.202890 11.00000 0.01569 0.03687 =
0.01704 -0.00019 0.00556 0.00018
C5 1 0.175211 0.681999 -0.233308 11.00000 0.02182 0.03658 =
0.01738 -0.00273 0.00637 -0.00136
C6 1 0.233092 0.669921 -0.178531 11.00000 0.02330 0.03657 =
0.02032 -0.00223 0.00976 0.00333
C7 1 0.263246 0.628051 -0.209635 11.00000 0.02970 0.04587 =
0.02486 -0.01003 0.01363 0.00157
AFIX 43
H7 2 0.247721 0.605606 -0.271223 11.00000 -1.20000
AFIX 0
C8 1 0.317479 0.626758 -0.135052 11.00000 0.02714 0.04335 =
0.03032 -0.00331 0.01643 0.00776
AFIX 43
H8 2 0.347259 0.603234 -0.134405 11.00000 -1.20000
AFIX 0
C9 1 0.322019 0.667518 -0.056598 11.00000 0.02089 0.03554 =
0.02381 0.00061 0.01198 0.00584
C10 1 0.370314 0.674217 0.037078 11.00000 0.01946 0.03886 =
0.02662 0.00365 0.01242 0.00806
C11 1 0.140093 0.649155 -0.333869 11.00000 0.02196 0.04873 =
0.01931 -0.00688 0.00730 0.00526
C12 1 0.130631 0.687191 -0.415135 11.00000 0.03749 0.05388 =
0.02366 -0.00394 0.01261 0.00716
C13 1 0.093977 0.657612 -0.507831 11.00000 0.04277 0.07053 =
0.02349 -0.00071 0.01367 0.01277
AFIX 43
H13 2 0.085836 0.683853 -0.563764 11.00000 -1.20000
AFIX 0
C14 1 0.069398 0.591773 -0.520438 11.00000 0.02940 0.06542 =
0.02726 -0.01608 0.00676 0.00795
C15 1 0.080457 0.554630 -0.439569 11.00000 0.02638 0.05548 =
0.03006 -0.01576 0.00862 0.00020
AFIX 43
H15 2 0.064024 0.508969 -0.447679 11.00000 -1.20000
AFIX 0
C16 1 0.115244 0.582190 -0.345634 11.00000 0.02227 0.05144 =
0.02669 -0.01237 0.00917 -0.00095
C17 1 0.157220 0.757564 -0.404118 11.00000 0.06829 0.06468 =
0.03000 0.00425 0.02128 -0.00362
AFIX 137
H17A 2 0.143960 0.791516 -0.375480 11.00000 -1.50000
H17B 2 0.147200 0.774854 -0.468215 11.00000 -1.50000
H17C 2 0.198069 0.752824 -0.361378 11.00000 -1.50000
AFIX 0
C18 1 0.030879 0.560642 -0.622152 11.00000 0.04938 0.08385 =
0.02517 -0.01945 0.00332 0.00644
AFIX 137
H18A 2 0.053232 0.546118 -0.648390 11.00000 -1.50000
H18B 2 0.003441 0.596687 -0.664913 11.00000 -1.50000
H18C 2 0.011194 0.519100 -0.618561 11.00000 -1.50000
AFIX 0
C19 1 0.123938 0.540514 -0.260387 11.00000 0.05037 0.05550 =
0.03619 -0.01230 0.01808 -0.01706
AFIX 137
H19A 2 0.163335 0.543877 -0.206361 11.00000 -1.50000
H19B 2 0.114192 0.490468 -0.279188 11.00000 -1.50000
H19C 2 0.099978 0.559923 -0.239817 11.00000 -1.50000
AFIX 0
C20 1 0.422119 0.634433 0.058963 11.00000 0.01912 0.04927 =
0.02486 -0.00130 0.00841 0.01071
C21 1 0.458187 0.660899 0.037050 11.00000 0.02716 0.03490 =
0.08444 -0.00839 0.03034 0.00012
AFIX 43
H21 2 0.450526 0.705295 0.004210 11.00000 -1.20000
AFIX 0
C22 1 0.507235 0.622676 0.062885 11.00000 0.02590 0.04641 =
0.09341 -0.01746 0.03291 -0.00681
AFIX 43
H22 2 0.532829 0.642327 0.048769 11.00000 -1.20000
AFIX 0
C23 1 0.518398 0.557919 0.107837 11.00000 0.02278 0.04725 =
0.02951 -0.01158 0.00266 0.00706
C24 1 0.482135 0.531681 0.126403 11.00000 0.08719 0.11215 =
0.13384 0.08406 0.08644 0.07179
AFIX 43
H24 2 0.488896 0.486110 0.156106 11.00000 -1.20000
AFIX 0
C25 1 0.434171 0.569216 0.103484 11.00000 0.08677 0.11805 =
0.14573 0.09780 0.09614 0.07924
AFIX 43
H25 2 0.409323 0.549156 0.119059 11.00000 -1.20000
AFIX 0
C26 1 0.568537 0.511501 0.130826 11.00000 0.02571 0.05452 =
0.04972 -0.02098 0.00752 0.00701
AFIX 23
H26A 2 0.554829 0.474741 0.079298 11.00000 -1.20000
H26B 2 0.581795 0.486340 0.192944 11.00000 -1.20000
AFIX 0
C27 1 0.666623 0.580084 0.267632 11.00000 0.04424 0.05027 =
0.04066 -0.01217 0.02387 -0.00240
AFIX 23
H27A 2 0.649176 0.622495 0.276570 11.00000 -1.20000
H27B 2 0.666661 0.540905 0.308190 11.00000 -1.20000
AFIX 0
C28 1 0.726792 0.597225 0.298514 11.00000 0.03161 0.04964 =
0.03409 -0.00515 0.01485 0.00122
AFIX 23
H28A 2 0.726435 0.638668 0.260735 11.00000 -1.20000
H28B 2 0.742514 0.556064 0.283287 11.00000 -1.20000
AFIX 0
C29 1 0.772117 0.530960 0.481908 11.00000 0.02785 0.04344 =
0.03729 -0.00528 0.01720 -0.00284
C30 1 0.803800 0.472303 0.488688 11.00000 0.04514 0.05118 =
0.06274 0.00658 0.03927 0.00700
AFIX 43
H30 2 0.828318 0.475595 0.466313 11.00000 -1.20000
AFIX 0
C31 1 0.799766 0.408880 0.528046 11.00000 0.07693 0.05116 =
0.11286 0.01623 0.07162 0.01708
AFIX 43
H31 2 0.821802 0.369122 0.532766 11.00000 -1.20000
AFIX 0
C32 1 0.764180 0.402802 0.560406 11.00000 0.08385 0.05297 =
0.10197 0.01729 0.07029 0.00446
AFIX 43
H32 2 0.761752 0.359255 0.587505 11.00000 -1.20000
AFIX 0
C33 1 0.732347 0.460319 0.553023 11.00000 0.06591 0.05945 =
0.08704 -0.00083 0.06144 -0.00367
AFIX 43
H33 2 0.707348 0.456403 0.574320 11.00000 -1.20000
AFIX 0
C34 1 0.736375 0.523382 0.515128 11.00000 0.03688 0.05191 =
0.05742 -0.00535 0.03118 -0.00096
AFIX 43
H34 2 0.714365 0.562871 0.511344 11.00000 -1.20000
AFIX 0
C35 1 0.841992 0.623187 0.449989 11.00000 0.02796 0.03866 =
0.04200 -0.00280 0.01934 0.00033
C36 1 0.851105 0.633895 0.375396 11.00000 0.03872 0.06161 =
0.04478 -0.00750 0.02539 -0.00628
AFIX 43
H36 2 0.820246 0.633689 0.309402 11.00000 -1.20000
AFIX 0
C37 1 0.904801 0.644818 0.396882 11.00000 0.04986 0.07093 =
0.06554 -0.01236 0.04159 -0.00747
AFIX 43
H37 2 0.910589 0.651994 0.345516 11.00000 -1.20000
AFIX 0
C38 1 0.949926 0.645370 0.492136 11.00000 0.03524 0.04828 =
0.08021 -0.01187 0.03599 -0.00411
AFIX 43
H38 2 0.986713 0.652789 0.506358 11.00000 -1.20000
AFIX 0
C39 1 0.941703 0.635179 0.566625 11.00000 0.02914 0.04187 =
0.05625 -0.00583 0.01737 0.00107
AFIX 43
H39 2 0.972789 0.635376 0.632424 11.00000 -1.20000
AFIX 0
C40 1 0.887668 0.624559 0.545412 11.00000 0.03120 0.04565 =
0.04209 -0.00133 0.01934 0.00150
AFIX 43
H40 2 0.882107 0.618172 0.597165 11.00000 -1.20000
AFIX 0
HKLF 4
REM n3163 in C2/c
REM R1 = 0.0541 for 5371 Fo > 4sig(Fo) and 0.0608 for all 6214 data
REM 406 parameters refined using 0 restraints
END
WGHT 0.1006 12.2145
REM Highest difference peak 0.829, deepest hole -0.614, 1-sigma level 0.077
Q1 1 0.6288 0.5824 0.2235 11.00000 0.05 0.83
Q2 1 0.5792 0.5544 0.0983 11.00000 0.05 0.55
Q3 1 0.7508 0.5962 0.3616 11.00000 0.05 0.53
Q4 1 0.7618 0.5413 0.3474 11.00000 0.05 0.51
Q5 1 0.1577 0.6668 -0.2776 11.00000 0.05 0.46
Q6 1 0.6306 0.5226 0.2438 11.00000 0.05 0.45
Q7 1 0.4421 0.5844 0.1396 11.00000 0.05 0.45
Q8 1 0.4527 0.5991 0.1026 11.00000 0.05 0.43
Q9 1 0.6054 0.5166 0.1593 11.00000 0.05 0.43
Q10 1 0.0770 0.7522 -0.2375 11.00000 0.05 0.42
Q11 1 0.3967 0.6537 0.0447 11.00000 0.05 0.42
Q12 1 0.4157 0.5621 0.0596 11.00000 0.05 0.40
Q13 1 0.1163 0.7319 -0.2348 11.00000 0.05 0.40
Q14 1 0.7519 0.5640 0.4044 11.00000 0.05 0.40
Q15 1 0.1506 0.7628 -0.1066 11.00000 0.05 0.39
Q16 1 0.2442 0.6492 -0.1907 11.00000 0.05 0.39
Q17 1 0.1273 0.7994 -0.0819 11.00000 0.05 0.38
Q18 1 0.1352 0.6132 -0.3374 11.00000 0.05 0.38
Q19 1 0.4943 0.6603 0.0046 11.00000 0.05 0.37
Q20 1 0.5010 0.5765 0.1222 11.00000 0.05 0.36
;
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3 7 5 29.44 0.31
3 7 6 0.72 0.06
3 7 7 1.81 0.07
3 7 8 10.52 0.21
3 7 9 12.42 0.27
3 7 10 0.63 0.07
3 7 11 0.59 0.08
3 7 12 1.11 0.09
3 7 13 0.22 0.08
3 7 14 0.31 0.11
3 9 0 11.95 0.14
3 9 1 9.95 0.27
3 9 2 0.61 0.06
3 9 3 6.61 0.12
3 9 4 20.43 0.21
3 9 5 34.26 0.38
3 9 6 21.02 0.28
3 9 7 12.73 0.21
3 9 8 5.76 0.16
3 9 9 18.92 0.32
3 9 10 0.95 0.10
3 9 11 0.58 0.08
3 9 12 1.96 0.12
3 9 13 0.02 0.12
3 11 0 0.03 0.05
3 11 1 5.42 0.18
3 11 2 1.84 0.06
3 11 3 6.61 0.14
3 11 4 0.53 0.05
3 11 5 27.12 0.31
3 11 6 0.15 0.04
3 11 7 23.30 0.31
3 11 8 13.39 0.25
3 11 9 2.27 0.10
3 11 10 1.39 0.10
3 11 11 0.48 0.08
3 11 12 0.53 0.12
3 13 0 4.69 0.15
3 13 1 4.36 0.14
3 13 2 0.06 0.06
3 13 3 3.47 0.15
3 13 4 0.93 0.06
3 13 5 3.00 0.08
3 13 6 11.41 0.19
3 13 7 3.65 0.13
3 13 8 0.59 0.08
3 13 9 6.57 0.20
3 13 10 0.54 0.09
3 13 11 3.88 0.27
3 13 12 2.01 0.17
3 15 0 0.58 0.07
3 15 1 19.16 0.33
3 15 2 0.51 0.08
3 15 3 0.06 0.06
3 15 4 0.44 0.06
3 15 5 0.07 0.06
3 15 6 0.30 0.08
3 15 7 0.03 0.09
3 15 8 5.19 0.17
3 15 9 0.00 0.08
3 15 10 0.00 0.08
3 17 0 0.10 0.06
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3 17 4 0.04 0.06
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3 17 8 1.51 0.13
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3 19 3 0.46 0.08
3 19 4 1.85 0.08
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3 19 7 2.18 0.28
3 21 0 1.10 0.08
3 21 1 2.30 0.12
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3 21 3 0.29 0.27
4 0 0 5.73 0.76
4 0 2 649.77 22.49
4 0 4 393.88 12.33
4 0 6 24.33 1.20
4 0 8 0.43 0.07
4 0 10 25.92 0.76
4 0 12 7.94 0.31
4 0 14 2.32 0.15
4 2 0 65.86 1.67
4 2 1 2.04 0.27
4 2 2 1.20 0.17
4 2 3 12.72 0.25
4 2 4 30.34 0.77
4 2 5 19.18 0.76
4 2 6 53.13 4.69
4 2 7 5.07 0.17
4 2 8 3.85 0.10
4 2 9 1.78 0.08
4 2 10 10.38 0.22
4 2 11 5.83 0.16
4 2 12 4.85 0.16
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4 4 3 27.71 0.50
4 4 4 0.10 0.05
4 4 5 75.46 1.05
4 4 6 69.65 1.11
4 4 7 0.83 0.05
4 4 8 21.54 0.24
4 4 9 0.59 0.06
4 4 10 2.03 0.10
4 4 11 0.51 0.06
4 4 12 15.55 0.32
4 4 13 1.48 0.10
4 4 14 2.24 0.13
4 6 0 8.87 0.15
4 6 1 5.71 0.43
4 6 2 30.07 0.42
4 6 3 7.06 0.16
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4 6 6 1.25 0.08
4 6 7 1.27 0.07
4 6 8 0.59 0.04
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4 8 3 1.31 0.14
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4 8 5 3.06 0.10
4 8 6 32.79 0.34
4 8 7 5.74 0.14
4 8 8 2.14 0.08
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4 8 10 1.61 0.10
4 8 11 0.03 0.07
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4 10 3 0.55 0.08
4 10 4 15.22 0.23
4 10 5 13.86 0.17
4 10 6 14.98 0.21
4 10 7 31.83 0.38
4 10 8 14.00 0.29
4 10 9 1.75 0.11
4 10 10 9.14 0.20
4 10 11 0.74 0.10
4 10 12 0.15 0.07
4 12 0 0.21 0.07
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4 12 4 0.54 0.04
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4 12 9 0.06 0.08
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4 12 11 1.08 0.10
4 12 12 1.25 0.16
4 14 0 26.60 0.39
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4 14 3 0.04 0.06
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4 14 11 0.09 0.12
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4 20 3 0.12 0.06
4 20 4 0.24 0.19
4 20 5 0.74 0.21
5 1 0 34.26 0.38
5 1 1 291.44 6.81
5 1 2 14.64 0.29
5 1 3 84.74 1.20
5 1 4 4.54 0.15
5 1 5 62.79 2.04
5 1 6 4.78 0.24
5 1 7 5.55 0.17
5 1 8 0.02 0.04
5 1 9 0.04 0.06
5 1 10 0.00 0.06
5 1 11 7.81 0.19
5 1 12 3.39 0.12
5 1 13 5.45 0.14
5 1 14 4.08 0.53
5 3 0 43.17 0.67
5 3 1 0.57 0.23
5 3 2 1.19 0.07
5 3 3 6.30 0.16
5 3 4 1.38 0.09
5 3 5 14.64 0.36
5 3 6 24.29 0.45
5 3 7 1.47 0.07
5 3 8 0.45 0.06
5 3 9 1.34 0.09
5 3 10 3.47 0.11
5 3 11 27.05 0.38
5 3 12 0.66 0.06
5 3 13 7.41 0.41
5 3 14 0.13 0.12
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5 5 1 26.26 0.86
5 5 2 0.64 0.07
5 5 3 0.20 0.06
5 5 4 23.52 0.57
5 5 5 2.58 0.07
5 5 6 0.14 0.04
5 5 7 35.01 0.40
5 5 8 2.08 0.07
5 5 9 31.01 0.38
5 5 10 4.18 0.12
5 5 11 0.18 0.08
5 5 12 3.75 0.14
5 5 13 5.79 0.17
5 7 0 4.87 0.11
5 7 1 1.94 0.17
5 7 2 3.38 0.12
5 7 3 8.79 0.17
5 7 4 18.44 0.32
5 7 5 9.66 0.16
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5 7 8 0.69 0.07
5 7 9 0.38 0.06
5 7 10 0.65 0.08
5 7 11 0.28 0.09
5 7 12 1.66 0.10
5 7 13 0.93 0.16
5 9 0 3.59 0.09
5 9 1 42.52 0.63
5 9 2 7.82 0.22
5 9 3 5.92 0.12
5 9 4 2.69 0.08
5 9 5 67.89 0.73
5 9 6 22.72 0.31
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5 9 8 0.24 0.09
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5 9 10 6.63 0.19
5 9 11 0.12 0.08
5 9 12 0.13 0.11
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5 13 8 1.18 0.11
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6 0 0 281.04 6.00
6 0 2 27.49 1.18
6 0 4 394.64 17.01
6 0 6 70.37 4.01
6 0 8 11.61 0.68
6 0 10 2.17 0.20
6 0 12 28.42 0.63
6 2 0 2.65 0.24
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6 2 2 14.41 0.32
6 2 3 0.62 0.05
6 2 4 8.59 0.40
6 2 5 3.57 0.16
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6 2 10 14.72 0.28
6 2 11 10.94 0.25
6 2 12 1.79 0.09
6 2 13 4.43 0.19
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6 4 3 0.02 0.07
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6 4 11 0.98 0.11
6 4 12 11.14 0.30
6 4 13 0.68 0.10
6 6 0 4.70 0.10
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6 6 8 1.89 0.08
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6 6 12 3.94 0.14
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6 8 2 33.40 0.64
6 8 3 0.17 0.06
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7 1 1 73.55 1.22
7 1 2 23.95 0.40
7 1 3 148.41 2.39
7 1 4 1.17 0.14
7 1 5 6.95 0.41
7 1 6 1.74 0.10
7 1 7 0.03 0.04
7 1 8 5.52 0.17
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7 3 11 5.35 0.16
7 3 12 6.44 0.22
7 3 13 6.37 0.21
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7 5 4 0.21 0.04
7 5 5 0.52 0.04
7 5 6 5.52 0.09
7 5 7 11.42 0.18
7 5 8 6.04 0.15
7 5 9 34.38 0.50
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7 5 12 1.15 0.10
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7 7 2 0.18 0.06
7 7 3 51.19 0.68
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7 7 8 6.28 0.15
7 7 9 5.03 0.16
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8 2 8 1.83 0.11
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9 1 4 0.25 0.11
9 1 5 96.70 1.34
9 1 6 10.88 0.24
9 1 7 0.01 0.06
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9 1 9 0.30 0.09
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9 5 8 0.40 0.08
9 5 9 0.03 0.07
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9 9 6 9.90 0.18
9 9 7 8.21 0.19
9 9 8 0.00 0.07
9 9 9 5.77 0.19
9 9 10 4.06 0.17
9 9 11 5.33 0.35
9 11 0 6.80 0.11
9 11 1 2.10 0.09
9 11 2 8.72 0.18
9 11 3 10.89 0.19
9 11 4 9.12 0.17
9 11 5 11.39 0.24
9 11 6 0.07 0.07
9 11 7 0.25 0.08
9 11 8 0.57 0.08
9 11 9 1.91 0.12
9 11 10 3.40 0.32
9 13 0 3.91 0.15
9 13 1 37.15 0.37
9 13 2 1.80 0.19
9 13 3 7.89 0.28
9 13 4 1.42 0.12
9 13 5 0.31 0.08
9 13 6 0.19 0.10
9 13 7 2.35 0.16
9 13 8 1.22 0.14
9 13 9 14.62 0.67
9 15 0 5.96 0.20
9 15 1 0.35 0.06
9 15 2 0.27 0.07
9 15 3 5.39 0.19
9 15 4 2.33 0.16
9 15 5 4.46 0.17
9 15 6 2.04 0.25
9 15 7 3.07 0.24
9 15 8 0.25 0.16
9 17 0 1.15 0.08
9 17 1 6.15 0.16
9 17 2 7.64 0.24
9 17 3 0.53 0.11
9 17 4 1.88 0.17
9 17 5 0.13 0.16
9 17 6 5.04 0.39
9 19 0 0.10 0.07
9 19 1 0.08 0.06
9 19 2 2.38 0.16
9 19 3 3.51 0.49
9 19 4 2.09 0.28
10 0 0 222.69 4.96
10 0 2 94.73 4.00
10 0 4 17.78 0.48
10 0 6 10.21 0.39
10 0 8 0.10 0.14
10 0 10 6.37 0.22
10 0 12 2.12 0.25
10 2 0 72.69 1.10
10 2 1 39.60 0.74
10 2 2 13.31 0.51
10 2 3 0.54 0.06
10 2 4 9.00 0.18
10 2 5 7.84 0.14
10 2 6 8.08 0.13
10 2 7 0.04 0.06
10 2 8 3.61 0.14
10 2 9 20.62 0.37
10 2 10 3.52 0.12
10 2 11 1.15 0.12
10 2 12 4.04 0.23
10 4 0 8.23 0.19
10 4 1 13.83 0.22
10 4 2 15.00 0.32
10 4 3 0.30 0.05
10 4 4 0.67 0.06
10 4 5 7.51 0.15
10 4 6 5.04 0.10
10 4 7 0.02 0.05
10 4 8 17.57 0.33
10 4 9 1.14 0.09
10 4 10 21.85 0.35
10 4 11 0.54 0.11
10 6 0 7.44 0.12
10 6 1 6.89 0.19
10 6 2 55.42 0.67
10 6 3 4.11 0.09
10 6 4 8.58 0.15
10 6 5 15.24 0.32
10 6 6 0.00 0.05
10 6 7 5.53 0.13
10 6 8 21.78 0.34
10 6 9 0.02 0.07
10 6 10 17.71 0.31
10 6 11 0.28 0.10
10 8 0 22.10 0.28
10 8 1 9.10 0.18
10 8 2 3.61 0.11
10 8 3 0.15 0.06
10 8 4 28.29 0.32
10 8 5 3.00 0.13
10 8 6 29.89 0.40
10 8 7 0.73 0.09
10 8 8 1.72 0.12
10 8 9 0.80 0.10
10 8 10 0.22 0.10
10 10 0 8.61 0.16
10 10 1 15.11 0.16
10 10 2 21.64 0.29
10 10 3 0.23 0.08
10 10 4 0.74 0.10
10 10 5 0.12 0.07
10 10 6 0.14 0.07
10 10 7 3.36 0.17
10 10 8 6.44 0.24
10 10 9 3.31 0.15
10 10 10 7.13 0.43
10 12 0 5.72 0.13
10 12 1 5.81 0.11
10 12 2 0.04 0.07
10 12 3 4.71 0.14
10 12 4 0.86 0.10
10 12 5 1.06 0.11
10 12 6 1.58 0.14
10 12 7 0.07 0.10
10 12 8 3.06 0.21
10 12 9 0.27 0.18
10 14 0 0.84 0.07
10 14 1 8.42 0.20
10 14 2 7.59 0.18
10 14 3 0.61 0.09
10 14 4 4.99 0.19
10 14 5 1.71 0.14
10 14 6 0.11 0.09
10 14 7 0.15 0.11
10 14 8 0.10 0.16
10 16 0 1.72 0.10
10 16 1 7.38 0.17
10 16 2 18.83 0.38
10 16 3 5.95 0.24
10 16 4 2.02 0.14
10 16 5 9.17 0.30
10 16 6 0.03 0.12
10 18 0 1.10 0.09
10 18 1 0.11 0.06
10 18 2 2.30 0.13
10 18 3 0.74 0.17
10 18 4 0.79 0.15
10 20 0 0.23 0.20
10 20 1 1.09 0.16
11 1 0 0.87 0.08
11 1 1 54.43 1.04
11 1 2 1.82 0.08
11 1 3 0.31 0.06
11 1 4 7.10 0.17
11 1 5 57.44 0.92
11 1 6 2.32 0.13
11 1 7 2.31 0.14
11 1 8 4.06 0.18
11 1 9 3.44 0.18
11 1 10 0.32 0.06
11 1 11 0.17 0.09
11 3 0 17.11 0.29
11 3 1 4.31 0.09
11 3 2 8.36 0.20
11 3 3 5.23 0.13
11 3 4 14.71 0.23
11 3 5 1.42 0.09
11 3 6 0.05 0.05
11 3 7 0.01 0.06
11 3 8 15.86 0.28
11 3 9 19.85 0.47
11 3 10 3.96 0.17
11 3 11 9.29 0.27
11 5 0 35.21 0.47
11 5 1 32.38 0.32
11 5 2 0.91 0.05
11 5 3 1.38 0.06
11 5 4 9.76 0.14
11 5 5 14.86 0.25
11 5 6 9.02 0.20
11 5 7 32.00 0.43
11 5 8 0.62 0.08
11 5 9 15.17 0.27
11 5 10 4.00 0.16
11 5 11 2.74 0.21
11 7 0 31.39 0.33
11 7 1 39.92 0.38
11 7 2 9.53 0.14
11 7 3 37.94 0.40
11 7 4 15.92 0.23
11 7 5 13.78 0.24
11 7 6 2.59 0.12
11 7 7 3.42 0.14
11 7 8 2.47 0.14
11 7 9 1.13 0.11
11 7 10 1.11 0.10
11 9 0 25.76 0.33
11 9 1 19.44 0.21
11 9 2 28.93 0.34
11 9 3 34.30 0.46
11 9 4 2.05 0.12
11 9 5 14.21 0.30
11 9 6 16.79 0.32
11 9 7 5.44 0.20
11 9 8 0.82 0.11
11 9 9 1.64 0.12
11 9 10 0.48 0.16
11 11 0 6.60 0.14
11 11 1 2.04 0.07
11 11 2 7.53 0.18
11 11 3 17.44 0.27
11 11 4 0.00 0.07
11 11 5 4.03 0.16
11 11 6 0.12 0.08
11 11 7 0.38 0.10
11 11 8 3.95 0.18
11 11 9 7.60 0.44
11 13 0 1.64 0.07
11 13 1 0.40 0.07
11 13 2 2.04 0.11
11 13 3 4.10 0.13
11 13 4 0.24 0.09
11 13 5 0.11 0.10
11 13 6 1.83 0.16
11 13 7 0.08 0.11
11 13 8 0.96 0.22
11 15 0 0.02 0.06
11 15 1 17.35 0.28
11 15 2 0.55 0.09
11 15 3 2.55 0.14
11 15 4 0.08 0.10
11 15 5 1.48 0.13
11 15 6 0.01 0.10
11 15 7 0.75 0.20
11 17 0 1.37 0.09
11 17 1 14.59 0.31
11 17 2 0.19 0.10
11 17 3 1.60 0.15
11 17 4 5.38 0.51
11 17 5 0.67 0.19
11 19 0 0.99 0.14
11 19 1 0.42 0.17
11 19 2 1.80 0.18
12 0 0 60.18 1.36
12 0 2 30.34 0.85
12 0 4 131.24 2.66
12 0 6 3.88 0.30
12 0 8 0.17 0.17
12 0 10 4.66 0.18
12 2 0 77.33 1.38
12 2 1 9.37 0.19
12 2 2 1.77 0.12
12 2 3 0.14 0.05
12 2 4 9.69 0.16
12 2 5 11.20 0.20
12 2 6 2.21 0.11
12 2 7 0.19 0.07
12 2 8 11.69 0.28
12 2 9 0.20 0.09
12 2 10 0.00 0.07
12 2 11 0.01 0.12
12 4 0 17.55 0.31
12 4 1 0.67 0.06
12 4 2 18.88 0.24
12 4 3 3.11 0.10
12 4 4 9.53 0.15
12 4 5 22.39 0.31
12 4 6 0.11 0.05
12 4 7 0.03 0.07
12 4 8 13.98 0.28
12 4 9 0.13 0.07
12 4 10 12.50 0.28
12 6 0 27.24 0.31
12 6 1 0.31 0.04
12 6 2 5.98 0.11
12 6 3 8.45 0.16
12 6 4 41.54 0.50
12 6 5 11.74 0.22
12 6 6 0.21 0.06
12 6 7 6.66 0.16
12 6 8 3.75 0.14
12 6 9 6.74 0.20
12 6 10 0.77 0.12
12 8 0 90.79 0.92
12 8 1 10.69 0.17
12 8 2 29.56 0.33
12 8 3 2.94 0.07
12 8 4 0.17 0.06
12 8 5 1.78 0.09
12 8 6 8.30 0.22
12 8 7 7.30 0.23
12 8 8 12.87 0.41
12 8 9 2.28 0.15
12 10 0 9.38 0.15
12 10 1 6.14 0.13
12 10 2 8.14 0.18
12 10 3 3.00 0.12
12 10 4 1.84 0.11
12 10 5 18.66 0.33
12 10 6 0.28 0.09
12 10 7 5.90 0.22
12 10 8 4.48 0.17
12 10 9 0.12 0.17
12 12 0 9.39 0.16
12 12 1 0.00 0.07
12 12 2 5.12 0.16
12 12 3 0.60 0.09
12 12 4 1.19 0.11
12 12 5 0.03 0.09
12 12 6 0.48 0.11
12 12 7 0.30 0.12
12 12 8 8.93 0.50
12 14 0 5.56 0.14
12 14 1 0.89 0.09
12 14 2 6.59 0.18
12 14 3 0.26 0.08
12 14 4 2.95 0.16
12 14 5 9.80 0.43
12 14 6 2.51 0.24
12 14 7 0.22 0.16
12 16 0 7.13 0.19
12 16 1 7.40 0.21
12 16 2 8.46 0.23
12 16 3 0.01 0.12
12 16 4 3.10 0.18
12 16 5 0.24 0.12
12 18 0 3.74 0.17
12 18 1 1.16 0.12
12 18 2 0.05 0.14
12 18 3 5.58 0.29
13 1 0 0.57 0.05
13 1 1 4.49 0.11
13 1 2 6.30 0.13
13 1 3 24.16 0.33
13 1 4 0.30 0.07
13 1 5 11.28 0.28
13 1 6 2.08 0.14
13 1 7 7.41 0.23
13 1 8 4.64 0.18
13 1 9 4.10 0.13
13 1 10 2.47 0.13
13 3 0 19.11 0.30
13 3 1 0.10 0.04
13 3 2 34.22 0.42
13 3 3 21.94 0.33
13 3 4 0.24 0.06
13 3 5 0.36 0.05
13 3 6 0.29 0.06
13 3 7 0.00 0.05
13 3 8 1.22 0.15
13 3 9 1.11 0.11
13 3 10 0.01 0.07
13 5 0 1.90 0.07
13 5 1 12.97 0.20
13 5 2 12.68 0.18
13 5 3 4.12 0.10
13 5 4 4.55 0.17
13 5 5 0.44 0.06
13 5 6 12.85 0.27
13 5 7 35.65 0.50
13 5 8 0.08 0.07
13 5 9 14.46 0.28
13 5 10 0.31 0.22
13 7 0 2.59 0.06
13 7 1 2.07 0.05
13 7 2 0.28 0.06
13 7 3 56.26 0.63
13 7 4 9.24 0.17
13 7 5 9.58 0.23
13 7 6 0.31 0.07
13 7 7 18.41 0.34
13 7 8 1.01 0.10
13 7 9 0.78 0.11
13 9 0 0.00 0.05
13 9 1 7.14 0.14
13 9 2 2.16 0.08
13 9 3 3.81 0.16
13 9 4 1.96 0.12
13 9 5 2.35 0.11
13 9 6 21.50 0.42
13 9 7 18.39 0.43
13 9 8 0.16 0.09
13 9 9 2.08 0.22
13 11 0 1.79 0.09
13 11 1 0.02 0.06
13 11 2 6.62 0.19
13 11 3 11.20 0.23
13 11 4 6.86 0.20
13 11 5 4.41 0.27
13 11 6 0.14 0.10
13 11 7 1.15 0.11
13 11 8 0.00 0.16
13 13 0 0.27 0.06
13 13 1 2.62 0.11
13 13 2 1.57 0.09
13 13 3 6.17 0.21
13 13 4 0.67 0.11
13 13 5 2.32 0.27
13 13 6 0.49 0.15
13 13 7 0.98 0.20
13 15 0 2.57 0.20
13 15 1 9.16 0.34
13 15 2 0.34 0.10
13 15 3 0.23 0.11
13 15 4 1.82 0.20
13 15 5 5.53 0.23
13 17 0 6.23 0.22
13 17 1 3.54 0.19
13 17 2 0.35 0.16
13 17 3 0.09 0.23
13 19 0 3.35 0.20
13 19 1 1.39 0.25
14 0 0 0.00 0.08
14 0 2 13.28 0.35
14 0 4 165.62 3.90
14 0 6 37.82 1.18
14 0 8 5.86 0.29
14 0 10 0.00 0.17
14 2 0 22.38 0.32
14 2 1 38.51 0.52
14 2 2 64.12 0.80
14 2 3 10.56 0.20
14 2 4 1.18 0.07
14 2 5 0.37 0.08
14 2 6 0.23 0.08
14 2 7 0.38 0.08
14 2 8 9.57 0.32
14 2 9 0.26 0.08
14 2 10 2.28 0.22
14 4 0 7.04 0.13
14 4 1 0.04 0.04
14 4 2 3.01 0.09
14 4 3 24.16 0.32
14 4 4 1.16 0.08
14 4 5 2.56 0.08
14 4 6 1.09 0.09
14 4 7 0.03 0.07
14 4 8 2.32 0.12
14 4 9 0.61 0.08
14 6 0 0.94 0.07
14 6 1 11.06 0.15
14 6 2 0.89 0.06
14 6 3 0.29 0.05
14 6 4 0.44 0.07
14 6 5 1.30 0.09
14 6 6 9.72 0.21
14 6 7 0.28 0.08
14 6 8 3.02 0.13
14 6 9 7.55 0.27
14 8 0 1.60 0.07
14 8 1 3.01 0.10
14 8 2 40.74 0.50
14 8 3 0.01 0.06
14 8 4 0.95 0.08
14 8 5 4.13 0.16
14 8 6 15.76 0.33
14 8 7 3.31 0.14
14 8 8 4.16 0.20
14 10 0 10.93 0.16
14 10 1 3.66 0.13
14 10 2 0.80 0.08
14 10 3 7.80 0.20
14 10 4 3.56 0.15
14 10 5 1.01 0.11
14 10 6 8.12 0.27
14 10 7 0.48 0.10
14 10 8 0.42 0.16
14 12 0 22.70 0.31
14 12 1 11.34 0.22
14 12 2 0.01 0.08
14 12 3 0.70 0.10
14 12 4 0.52 0.11
14 12 5 1.59 0.14
14 12 6 1.12 0.21
14 12 7 1.01 0.19
14 14 0 6.50 0.20
14 14 1 1.27 0.10
14 14 2 0.00 0.09
14 14 3 2.90 0.15
14 14 4 3.77 0.16
14 14 5 0.00 0.09
14 14 6 6.36 0.41
14 16 0 1.29 0.12
14 16 1 2.18 0.16
14 16 2 0.02 0.12
14 16 3 2.29 0.18
14 16 4 6.06 0.27
14 18 0 2.17 0.20
14 18 1 4.26 0.28
15 1 0 12.47 0.18
15 1 1 63.67 0.71
15 1 2 17.97 0.36
15 1 3 97.74 1.56
15 1 4 8.26 0.20
15 1 5 15.34 0.33
15 1 6 1.12 0.11
15 1 7 11.74 0.30
15 1 8 1.90 0.19
15 1 9 0.99 0.10
15 3 0 2.35 0.08
15 3 1 1.73 0.06
15 3 2 11.67 0.18
15 3 3 7.68 0.17
15 3 4 11.78 0.21
15 3 5 4.64 0.13
15 3 6 0.00 0.05
15 3 7 14.59 0.35
15 3 8 2.60 0.14
15 3 9 0.07 0.07
15 5 0 2.72 0.07
15 5 1 2.09 0.07
15 5 2 36.46 0.43
15 5 3 1.50 0.09
15 5 4 0.06 0.05
15 5 5 17.54 0.29
15 5 6 2.93 0.12
15 5 7 0.03 0.06
15 5 8 4.97 0.18
15 5 9 18.03 0.81
15 7 0 0.14 0.04
15 7 1 0.09 0.04
15 7 2 32.49 0.46
15 7 3 0.00 0.06
15 7 4 8.74 0.20
15 7 5 10.20 0.22
15 7 6 3.06 0.14
15 7 7 18.38 0.31
15 7 8 4.01 0.16
15 9 0 0.06 0.05
15 9 1 17.39 0.27
15 9 2 3.60 0.11
15 9 3 0.02 0.06
15 9 4 2.82 0.13
15 9 5 14.90 0.34
15 9 6 3.73 0.16
15 9 7 11.27 0.29
15 9 8 8.32 0.43
15 11 0 4.68 0.13
15 11 1 5.46 0.18
15 11 2 18.42 0.34
15 11 3 1.23 0.09
15 11 4 0.08 0.08
15 11 5 0.33 0.11
15 11 6 0.82 0.13
15 11 7 0.00 0.13
15 13 0 2.34 0.10
15 13 1 3.91 0.15
15 13 2 8.14 0.26
15 13 3 0.03 0.09
15 13 4 0.66 0.10
15 13 5 5.75 0.49
15 13 6 0.00 0.14
15 15 0 1.10 0.13
15 15 1 1.06 0.20
15 15 2 1.98 0.17
15 15 3 5.33 0.36
15 15 4 0.00 0.12
15 17 0 13.77 0.33
15 17 1 0.12 0.15
15 17 2 1.98 0.18
16 0 0 37.37 0.55
16 0 2 5.95 0.16
16 0 4 11.25 0.37
16 0 6 55.12 1.23
16 0 8 12.58 0.29
16 2 0 0.13 0.04
16 2 1 23.61 0.34
16 2 2 23.14 0.32
16 2 3 20.95 0.28
16 2 4 11.09 0.24
16 2 5 8.13 0.21
16 2 6 3.15 0.13
16 2 7 3.14 0.15
16 2 8 0.88 0.10
16 2 9 14.61 0.70
16 4 0 15.82 0.21
16 4 1 0.21 0.04
16 4 2 3.87 0.11
16 4 3 4.10 0.12
16 4 4 0.57 0.06
16 4 5 0.47 0.07
16 4 6 6.86 0.18
16 4 7 0.97 0.10
16 4 8 3.89 0.15
16 6 0 2.57 0.10
16 6 1 40.93 0.42
16 6 2 5.13 0.11
16 6 3 17.46 0.31
16 6 4 0.39 0.07
16 6 5 5.67 0.19
16 6 6 21.46 0.38
16 6 7 0.27 0.07
16 6 8 12.52 0.50
16 8 0 2.84 0.09
16 8 1 2.72 0.09
16 8 2 7.37 0.15
16 8 3 1.37 0.08
16 8 4 10.09 0.22
16 8 5 5.73 0.19
16 8 6 13.36 0.43
16 8 7 0.11 0.07
16 10 0 4.48 0.11
16 10 1 10.41 0.22
16 10 2 1.70 0.09
16 10 3 12.98 0.24
16 10 4 0.50 0.12
16 10 5 0.12 0.10
16 10 6 4.55 0.21
16 10 7 0.23 0.15
16 12 0 1.11 0.09
16 12 1 2.23 0.14
16 12 2 1.28 0.13
16 12 3 0.86 0.11
16 12 4 6.54 0.29
16 12 5 0.18 0.19
16 12 6 0.00 0.13
16 14 0 0.20 0.08
16 14 1 1.77 0.13
16 14 2 0.82 0.10
16 14 3 1.15 0.14
16 14 4 11.64 0.60
16 16 0 0.96 0.17
16 16 1 0.00 0.14
16 16 2 0.01 0.15
16 18 0 0.27 0.14
17 1 0 5.31 0.10
17 1 1 0.40 0.04
17 1 2 17.74 0.32
17 1 3 6.43 0.19
17 1 4 1.92 0.12
17 1 5 30.03 0.56
17 1 6 5.85 0.21
17 1 7 8.63 0.36
17 1 8 1.09 0.11
17 3 0 0.10 0.04
17 3 1 106.28 1.19
17 3 2 0.69 0.07
17 3 3 0.39 0.06
17 3 4 2.35 0.10
17 3 5 2.64 0.11
17 3 6 0.56 0.10
17 3 7 0.83 0.09
17 3 8 1.39 0.13
17 5 0 6.79 0.13
17 5 1 0.42 0.06
17 5 2 47.92 0.63
17 5 3 3.81 0.12
17 5 4 0.72 0.07
17 5 5 17.99 0.30
17 5 6 0.03 0.06
17 5 7 0.05 0.08
17 5 8 5.88 0.39
17 7 0 2.50 0.12
17 7 1 14.99 0.26
17 7 2 1.38 0.09
17 7 3 1.21 0.09
17 7 4 2.12 0.11
17 7 5 3.99 0.14
17 7 6 0.65 0.08
17 7 7 6.11 0.22
17 9 0 1.61 0.07
17 9 1 5.38 0.14
17 9 2 12.04 0.22
17 9 3 0.00 0.06
17 9 4 0.45 0.09
17 9 5 2.53 0.13
17 9 6 1.58 0.18
17 11 0 4.54 0.14
17 11 1 1.63 0.09
17 11 2 8.49 0.22
17 11 3 7.82 0.20
17 11 4 2.39 0.15
17 11 5 3.28 0.25
17 13 0 1.80 0.12
17 13 1 1.44 0.14
17 13 2 0.00 0.09
17 13 3 7.15 0.23
17 13 4 0.93 0.17
17 15 0 0.24 0.11
17 15 1 0.61 0.12
17 15 2 0.72 0.14
17 15 3 6.08 0.37
17 17 0 0.29 0.13
18 0 0 1.00 0.07
18 0 2 19.35 0.39
18 0 4 11.08 0.39
18 0 6 5.32 0.24
18 2 0 7.35 0.14
18 2 1 0.09 0.05
18 2 2 8.15 0.22
18 2 3 0.44 0.07
18 2 4 27.07 0.47
18 2 5 0.18 0.08
18 2 6 17.31 0.38
18 2 7 1.82 0.11
18 4 0 40.76 0.49
18 4 1 13.36 0.27
18 4 2 7.84 0.17
18 4 3 3.30 0.10
18 4 4 9.49 0.18
18 4 5 0.01 0.06
18 4 6 0.00 0.08
18 4 7 0.81 0.08
18 6 0 2.97 0.09
18 6 1 2.50 0.09
18 6 2 6.61 0.20
18 6 3 6.89 0.21
18 6 4 2.92 0.13
18 6 5 0.96 0.08
18 6 6 0.32 0.07
18 6 7 12.81 0.63
18 8 0 0.60 0.07
18 8 1 0.14 0.06
18 8 2 7.02 0.17
18 8 3 2.95 0.13
18 8 4 8.19 0.22
18 8 5 0.03 0.07
18 8 6 16.34 0.39
18 10 0 16.81 0.27
18 10 1 3.41 0.13
18 10 2 3.08 0.13
18 10 3 10.31 0.26
18 10 4 0.07 0.09
18 10 5 0.92 0.11
18 12 0 2.55 0.13
18 12 1 0.08 0.10
18 12 2 3.88 0.17
18 12 3 0.98 0.13
18 12 4 7.11 0.39
18 14 0 0.55 0.13
18 14 1 0.05 0.11
18 14 2 1.93 0.24
18 14 3 0.38 0.17
18 16 0 0.27 0.14
19 1 0 13.58 0.29
19 1 1 2.48 0.09
19 1 2 1.98 0.09
19 1 3 12.49 0.23
19 1 4 2.13 0.11
19 1 5 10.43 0.27
19 1 6 0.16 0.08
19 1 7 10.04 0.28
19 3 0 1.57 0.12
19 3 1 5.84 0.16
19 3 2 2.65 0.11
19 3 3 25.16 0.42
19 3 4 2.37 0.14
19 3 5 2.79 0.13
19 3 6 0.09 0.07
19 3 7 0.18 0.15
19 5 0 0.61 0.08
19 5 1 1.83 0.10
19 5 2 8.38 0.20
19 5 3 0.10 0.07
19 5 4 0.30 0.07
19 5 5 3.74 0.13
19 5 6 0.01 0.08
19 7 0 0.29 0.06
19 7 1 19.32 0.32
19 7 2 14.36 0.28
19 7 3 27.35 0.47
19 7 4 0.06 0.07
19 7 5 8.34 0.33
19 7 6 0.35 0.10
19 9 0 0.54 0.07
19 9 1 0.97 0.08
19 9 2 16.90 0.32
19 9 3 1.90 0.12
19 9 4 0.40 0.08
19 9 5 1.58 0.22
19 11 0 6.98 0.21
19 11 1 4.17 0.17
19 11 2 0.04 0.10
19 11 3 1.92 0.17
19 11 4 0.53 0.18
19 13 0 0.00 0.10
19 13 1 1.45 0.13
19 13 2 0.40 0.19
19 13 3 10.04 0.50
19 15 0 5.03 0.25
19 15 1 0.11 0.17
20 0 0 55.38 0.90
20 0 2 17.94 0.75
20 0 4 32.36 0.75
20 0 6 23.69 0.71
20 2 0 24.81 0.43
20 2 1 0.76 0.08
20 2 2 8.11 0.22
20 2 3 0.02 0.07
20 2 4 1.41 0.10
20 2 5 0.22 0.07
20 2 6 3.57 0.16
20 4 0 3.36 0.12
20 4 1 20.32 0.30
20 4 2 2.26 0.09
20 4 3 4.60 0.14
20 4 4 8.16 0.20
20 4 5 0.26 0.09
20 4 6 0.59 0.17
20 6 0 0.53 0.07
20 6 1 5.92 0.17
20 6 2 4.62 0.21
20 6 3 0.45 0.08
20 6 4 6.13 0.18
20 6 5 5.12 0.16
20 8 0 28.68 0.40
20 8 1 12.98 0.24
20 8 2 4.78 0.17
20 8 3 0.06 0.08
20 8 4 0.08 0.07
20 8 5 2.99 0.25
20 10 0 4.59 0.15
20 10 1 0.32 0.07
20 10 2 10.74 0.24
20 10 3 4.27 0.20
20 10 4 2.13 0.25
20 12 0 10.22 0.25
20 12 1 1.65 0.13
20 12 2 0.71 0.21
20 12 3 0.81 0.20
20 14 0 1.16 0.16
20 14 1 0.14 0.17
21 1 0 3.90 0.12
21 1 1 2.57 0.13
21 1 2 0.01 0.05
21 1 3 11.79 0.25
21 1 4 1.79 0.10
21 1 5 7.42 0.21
21 3 0 0.65 0.07
21 3 1 0.00 0.06
21 3 2 3.10 0.12
21 3 3 13.54 0.25
21 3 4 3.19 0.15
21 3 5 6.85 0.19
21 5 0 3.61 0.13
21 5 1 33.09 0.50
21 5 2 0.78 0.08
21 5 3 1.65 0.10
21 5 4 4.85 0.16
21 5 5 0.08 0.08
21 7 0 0.03 0.07
21 7 1 1.02 0.09
21 7 2 8.25 0.21
21 7 3 11.70 0.26
21 7 4 0.15 0.07
21 9 0 0.07 0.07
21 9 1 3.51 0.14
21 9 2 6.86 0.20
21 9 3 3.71 0.17
21 9 4 0.00 0.12
21 11 0 4.03 0.16
21 11 1 9.42 0.41
21 11 2 0.12 0.17
21 11 3 0.19 0.15
21 13 0 4.23 0.28
21 13 1 2.41 0.28
22 0 0 7.04 0.19
22 0 2 2.51 0.22
22 0 4 6.65 0.23
22 2 0 0.10 0.06
22 2 1 6.45 0.17
22 2 2 18.82 0.30
22 2 3 7.57 0.19
22 2 4 3.61 0.17
22 2 5 0.01 0.14
22 4 0 32.65 0.41
22 4 1 0.21 0.06
22 4 2 5.16 0.19
22 4 3 1.51 0.09
22 4 4 0.37 0.09
22 6 0 25.45 0.47
22 6 1 7.79 0.23
22 6 2 7.96 0.23
22 6 3 5.49 0.20
22 6 4 4.64 0.23
22 8 0 3.25 0.14
22 8 1 0.62 0.09
22 8 2 18.06 0.37
22 8 3 0.99 0.11
22 10 0 1.04 0.11
22 10 1 0.28 0.10
22 10 2 0.37 0.18
22 12 0 5.74 0.41
22 12 1 0.32 0.17
23 1 0 5.39 0.15
23 1 1 4.96 0.23
23 1 2 1.72 0.10
23 1 3 6.52 0.17
23 1 4 0.85 0.09
23 3 0 3.51 0.11
23 3 1 16.36 0.26
23 3 2 0.51 0.07
23 3 3 0.60 0.08
23 3 4 0.00 0.10
23 5 0 3.32 0.14
23 5 1 8.79 0.23
23 5 2 3.51 0.14
23 5 3 3.77 0.16
23 7 0 1.47 0.13
23 7 1 2.18 0.12
23 7 2 4.01 0.16
23 7 3 0.71 0.15
23 9 0 0.69 0.09
23 9 1 2.00 0.13
23 9 2 0.29 0.15
23 11 0 0.44 0.13
23 11 1 7.06 0.40
24 0 0 1.76 0.13
24 0 2 0.97 0.13
24 2 0 8.32 0.17
24 2 1 2.99 0.10
24 2 2 9.43 0.21
24 2 3 0.28 0.07
24 4 0 24.71 0.40
24 4 1 2.45 0.11
24 4 2 5.94 0.25
24 4 3 1.90 0.32
24 6 0 9.71 0.25
24 6 1 3.23 0.15
24 6 2 0.44 0.09
24 8 0 2.56 0.21
24 8 1 0.10 0.13
24 8 2 2.58 0.23
24 10 0 15.56 0.50
25 1 0 0.44 0.06
25 1 1 0.21 0.06
25 1 2 2.27 0.14
25 3 0 3.48 0.11
25 3 1 17.42 0.27
25 3 2 0.31 0.10
25 5 0 0.83 0.09
25 5 1 1.63 0.12
25 7 0 1.15 0.12
25 7 1 1.51 0.15
25 9 0 0.11 0.14
26 0 0 1.69 0.22
26 2 0 6.47 0.21
26 2 1 0.30 0.08
26 4 0 11.31 0.41
26 4 1 0.04 0.09
26 6 0 1.19 0.12
26 8 0 1.32 0.19
27 1 0 6.53 0.19
27 3 0 2.36 0.35
27 5 0 2.29 0.20
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 41420
#===end
data_5
_audit_creation_date 2014-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number 2013-4
_publ_contact_author_address ?
_publ_contact_author_email ?
_publ_contact_author_name ''
_publ_contact_author_phone ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C31 H37 B F2 N3 P'
_chemical_formula_sum 'C31 H37 B F2 N3 P'
_chemical_formula_weight 531.41
_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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P' 'P' 0.2955 0.4335 '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/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 8.4508(4)
_cell_length_b 41.4961(16)
_cell_length_c 8.0700(3)
_cell_angle_alpha 90
_cell_angle_beta 94.122(4)
_cell_angle_gamma 90
_cell_volume 2822.6(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3948
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 64.752
_cell_measurement_theta_min 4.261
_shelx_estimated_absorpt_T_max 0.976
_shelx_estimated_absorpt_T_min 0.844
_exptl_absorpt_coefficient_mu 1.169
_exptl_absorpt_correction_T_max 0.9844
_exptl_absorpt_correction_T_min 0.9260
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
'A face indexed absorption correction was applied via XPREP'
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.251
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description 'plate'
_exptl_crystal_F_000 1128
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.098
_exptl_crystal_size_min 0.021
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0769
_diffrn_reflns_av_unetI/netI 0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 42
_diffrn_reflns_limit_k_min -48
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 10525
_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 63.703
_diffrn_reflns_theta_min 2.129
_diffrn_ambient_temperature 100.03
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3111
_reflns_number_total 4343
_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, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max 0.781
_refine_diff_density_min -0.398
_refine_diff_density_rms 0.075
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 353
_refine_ls_number_reflns 4343
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1133
_refine_ls_R_factor_gt 0.0838
_refine_ls_restrained_S_all 1.096
_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^)+(0.0764P)^2^+7.7468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2054
_refine_ls_wR_factor_ref 0.2168
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
C29(H29), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_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
P1 P 0.38396(17) 0.18908(3) 0.48769(17) 0.0258(4) Uani 1 1 d . . . . .
F1 F 1.0735(3) 0.09208(7) 0.4849(4) 0.0287(7) Uani 1 1 d . . . . .
F2 F 1.0728(4) 0.04626(7) 0.3329(4) 0.0306(7) Uani 1 1 d . . . . .
N1 N 0.8478(5) 0.05611(9) 0.4913(5) 0.0199(9) Uani 1 1 d . . . . .
N2 N 0.8884(5) 0.08785(10) 0.2392(5) 0.0227(10) Uani 1 1 d . . . . .
N3 N 0.4764(6) 0.09570(10) 0.3461(6) 0.0243(10) Uani 1 1 d . . . . .
H3 H 0.421(6) 0.0839(12) 0.405(6) 0.008(12) Uiso 1 1 d . . . . .
C1 C 0.8750(6) 0.03635(12) 0.6263(6) 0.0229(12) Uani 1 1 d . . . . .
C2 C 0.7280(6) 0.02832(13) 0.6876(7) 0.0271(12) Uani 1 1 d . . . . .
C3 C 0.6092(6) 0.04495(13) 0.5931(7) 0.0254(12) Uani 1 1 d . . . . .
C4 C 0.6873(6) 0.06229(12) 0.4721(6) 0.0199(11) Uani 1 1 d . . . . .
C5 C 0.6280(6) 0.08434(12) 0.3478(7) 0.0225(12) Uani 1 1 d . . . . .
C6 C 0.7286(6) 0.09463(12) 0.2227(6) 0.0206(11) Uani 1 1 d . . . . .
C7 C 0.6921(6) 0.10728(12) 0.0616(6) 0.0219(11) Uani 1 1 d . . . . .
C8 C 0.8340(7) 0.10873(12) -0.0156(6) 0.0252(12) Uani 1 1 d . . . . .
C9 C 0.9523(6) 0.09683(12) 0.0942(6) 0.0241(12) Uani 1 1 d . . . . .
C10 C 1.0364(6) 0.02696(13) 0.6929(7) 0.0271(12) Uani 1 1 d . . . . .
H10A H 1.0867 0.0138 0.6105 0.041 Uiso 1 1 calc GR . . . .
H10B H 1.0293 0.0145 0.7951 0.041 Uiso 1 1 calc GR . . . .
H10C H 1.1001 0.0464 0.7170 0.041 Uiso 1 1 calc GR . . . .
C11 C 0.7044(7) 0.00577(13) 0.8315(7) 0.0300(13) Uani 1 1 d . . . . .
H11A H 0.6071 -0.0071 0.8060 0.036 Uiso 1 1 calc R . . . .
H11B H 0.7953 -0.0093 0.8444 0.036 Uiso 1 1 calc R . . . .
C12 C 0.6903(7) 0.02345(14) 0.9922(7) 0.0359(14) Uani 1 1 d . . . . .
H12A H 0.5937 0.0366 0.9843 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.7830 0.0374 1.0143 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.6849 0.0079 1.0829 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.4353(7) 0.04311(14) 0.6151(7) 0.0310(13) Uani 1 1 d . . . . .
H13A H 0.3991 0.0637 0.6588 0.046 Uiso 1 1 calc GR . . . .
H13B H 0.4149 0.0258 0.6932 0.046 Uiso 1 1 calc GR . . . .
H13C H 0.3779 0.0387 0.5076 0.046 Uiso 1 1 calc GR . . . .
C14 C 0.5296(7) 0.11389(13) -0.0221(7) 0.0308(13) Uani 1 1 d . . . . .
H14A H 0.4503 0.1010 0.0312 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.5286 0.1081 -0.1399 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.5046 0.1368 -0.0118 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.8525(7) 0.12065(14) -0.1899(7) 0.0298(13) Uani 1 1 d . . . . .
H15A H 0.7726 0.1100 -0.2673 0.036 Uiso 1 1 calc R . . . .
H15B H 0.9590 0.1146 -0.2235 0.036 Uiso 1 1 calc R . . . .
C16 C 0.8326(8) 0.15673(15) -0.2035(7) 0.0380(15) Uani 1 1 d . . . . .
H16A H 0.8514 0.1637 -0.3164 0.057 Uiso 1 1 calc GR . . . .
H16B H 0.9088 0.1673 -0.1240 0.057 Uiso 1 1 calc GR . . . .
H16C H 0.7245 0.1626 -0.1787 0.057 Uiso 1 1 calc GR . . . .
C17 C 1.1228(6) 0.09260(14) 0.0650(7) 0.0304(13) Uani 1 1 d . . . . .
H17A H 1.1833 0.0884 0.1710 0.046 Uiso 1 1 calc GR . . . .
H17B H 1.1628 0.1123 0.0152 0.046 Uiso 1 1 calc GR . . . .
H17C H 1.1348 0.0744 -0.0104 0.046 Uiso 1 1 calc GR . . . .
C18 C 0.4399(7) 0.13049(13) 0.3306(7) 0.0265(12) Uani 1 1 d . . . . .
H18A H 0.3434 0.1335 0.2552 0.032 Uiso 1 1 calc R . . . .
H18B H 0.5288 0.1417 0.2818 0.032 Uiso 1 1 calc R . . . .
C19 C 0.4136(7) 0.14495(12) 0.4995(7) 0.0270(12) Uani 1 1 d . . . . .
H19A H 0.5066 0.1402 0.5773 0.032 Uiso 1 1 calc R . . . .
H19B H 0.3194 0.1348 0.5438 0.032 Uiso 1 1 calc R . . . .
C20 C 0.3794(7) 0.19778(12) 0.7104(6) 0.0266(12) Uani 1 1 d . . . . .
C21 C 0.5088(7) 0.21473(13) 0.7828(7) 0.0306(13) Uani 1 1 d . . . . .
H21 H 0.5903 0.2218 0.7160 0.037 Uiso 1 1 calc R . . . .
C22 C 0.5197(8) 0.22144(13) 0.9517(7) 0.0334(14) Uani 1 1 d . . . . .
H22 H 0.6082 0.2330 1.0005 0.040 Uiso 1 1 calc R . . . .
C23 C 0.4012(8) 0.21126(13) 1.0481(7) 0.0351(15) Uani 1 1 d . . . . .
H23 H 0.4083 0.2160 1.1636 0.042 Uiso 1 1 calc R . . . .
C24 C 0.2717(8) 0.19420(13) 0.9786(7) 0.0347(14) Uani 1 1 d . . . . .
H24 H 0.1907 0.1870 1.0456 0.042 Uiso 1 1 calc R . . . .
C25 C 0.2625(7) 0.18772(13) 0.8083(7) 0.0298(13) Uani 1 1 d . . . . .
H25 H 0.1740 0.1762 0.7594 0.036 Uiso 1 1 calc R . . . .
C26 C 0.1723(7) 0.19336(13) 0.4197(7) 0.0288(13) Uani 1 1 d . . . . .
C27 C 0.0673(7) 0.16826(13) 0.3820(7) 0.0297(13) Uani 1 1 d . . . . .
H27 H 0.1028 0.1466 0.3946 0.036 Uiso 1 1 calc R . . . .
C28 C -0.0876(7) 0.17432(14) 0.3265(7) 0.0349(14) Uani 1 1 d . . . . .
H28 H -0.1577 0.1568 0.3027 0.042 Uiso 1 1 calc R . . . .
C29 C -0.1435(8) 0.20566(16) 0.3046(9) 0.0491(18) Uani 1 1 d . . . . .
H29 H -0.2511 0.2098 0.2688 0.059 Uiso 1 1 calc R . . . .
C30 C -0.0364(9) 0.23067(16) 0.3370(11) 0.061(2) Uani 1 1 d . . . . .
H30 H -0.0708 0.2524 0.3230 0.073 Uiso 1 1 calc R . . . .
C31 C 0.1190(8) 0.22428(15) 0.3890(9) 0.0498(19) Uani 1 1 d . . . . .
H31 H 0.1915 0.2417 0.4042 0.060 Uiso 1 1 calc R . . . .
B1 B 0.9772(7) 0.07073(13) 0.3876(7) 0.0209(13) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0346(8) 0.0209(7) 0.0215(7) -0.0011(5) 0.0000(6) 0.0002(6)
F1 0.0287(17) 0.0258(16) 0.0305(17) 0.0036(13) -0.0058(13) -0.0066(13)
F2 0.0285(17) 0.0256(16) 0.0386(18) 0.0041(13) 0.0083(14) 0.0070(13)
N1 0.019(2) 0.016(2) 0.024(2) 0.0016(17) -0.0011(18) 0.0005(17)
N2 0.026(2) 0.018(2) 0.024(2) 0.0007(18) 0.0045(19) -0.0007(18)
N3 0.028(3) 0.018(2) 0.028(3) 0.0034(19) 0.005(2) -0.002(2)
C1 0.025(3) 0.020(3) 0.024(3) 0.000(2) 0.003(2) -0.004(2)
C2 0.026(3) 0.025(3) 0.030(3) -0.001(2) 0.002(2) -0.006(2)
C3 0.023(3) 0.024(3) 0.029(3) -0.001(2) -0.001(2) -0.003(2)
C4 0.020(3) 0.019(3) 0.021(3) -0.002(2) 0.004(2) -0.005(2)
C5 0.017(3) 0.017(3) 0.033(3) -0.001(2) -0.004(2) -0.003(2)
C6 0.027(3) 0.017(3) 0.018(3) -0.001(2) 0.001(2) -0.005(2)
C7 0.019(3) 0.018(3) 0.028(3) -0.005(2) -0.001(2) -0.004(2)
C8 0.032(3) 0.020(3) 0.024(3) -0.004(2) 0.003(2) -0.001(2)
C9 0.032(3) 0.020(3) 0.021(3) 0.000(2) -0.001(2) 0.003(2)
C10 0.027(3) 0.027(3) 0.027(3) 0.006(2) 0.001(2) -0.003(2)
C11 0.024(3) 0.028(3) 0.037(3) 0.005(2) 0.002(2) 0.001(2)
C12 0.035(3) 0.031(3) 0.042(4) 0.008(3) 0.002(3) -0.004(3)
C13 0.027(3) 0.034(3) 0.032(3) 0.011(2) 0.005(2) 0.000(2)
C14 0.038(3) 0.027(3) 0.028(3) -0.005(2) 0.004(3) -0.005(3)
C15 0.029(3) 0.038(3) 0.023(3) 0.002(2) 0.001(2) 0.003(2)
C16 0.046(4) 0.041(4) 0.028(3) 0.011(3) 0.009(3) 0.000(3)
C17 0.023(3) 0.038(3) 0.030(3) 0.001(2) -0.003(2) -0.001(2)
C18 0.027(3) 0.024(3) 0.028(3) -0.001(2) 0.004(2) 0.004(2)
C19 0.029(3) 0.024(3) 0.028(3) 0.000(2) -0.001(2) 0.004(2)
C20 0.041(3) 0.018(3) 0.021(3) 0.001(2) 0.000(2) 0.006(2)
C21 0.036(3) 0.021(3) 0.034(3) 0.001(2) -0.002(3) 0.003(2)
C22 0.046(4) 0.026(3) 0.026(3) -0.003(2) -0.010(3) 0.002(3)
C23 0.057(4) 0.026(3) 0.021(3) -0.004(2) -0.003(3) 0.004(3)
C24 0.053(4) 0.025(3) 0.027(3) 0.004(2) 0.008(3) 0.008(3)
C25 0.036(3) 0.022(3) 0.032(3) -0.002(2) 0.003(3) 0.002(2)
C26 0.038(3) 0.021(3) 0.028(3) 0.000(2) 0.001(2) -0.001(2)
C27 0.032(3) 0.021(3) 0.036(3) 0.004(2) 0.002(3) 0.003(2)
C28 0.038(4) 0.027(3) 0.040(4) -0.003(3) 0.004(3) -0.007(3)
C29 0.039(4) 0.045(4) 0.060(4) 0.005(3) -0.019(3) 0.002(3)
C30 0.049(5) 0.025(3) 0.104(6) -0.002(4) -0.026(4) 0.000(3)
C31 0.044(4) 0.024(3) 0.077(5) -0.003(3) -0.024(4) -0.001(3)
B1 0.029(3) 0.012(3) 0.022(3) 0.001(2) -0.001(3) -0.004(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
P1 C19 1.850(5) . ?
P1 C20 1.836(5) . ?
P1 C26 1.841(6) . ?
F1 B1 1.404(6) . ?
F2 B1 1.389(7) . ?
N1 C1 1.369(6) . ?
N1 C4 1.379(6) . ?
N1 B1 1.548(7) . ?
N2 C6 1.376(7) . ?
N2 C9 1.375(7) . ?
N2 B1 1.541(7) . ?
N3 H3 0.85(5) . ?
N3 C5 1.364(7) . ?
N3 C18 1.479(7) . ?
C1 C2 1.410(8) . ?
C1 C10 1.482(7) . ?
C2 C3 1.398(8) . ?
C2 C11 1.516(8) . ?
C3 C4 1.414(8) . ?
C3 C13 1.495(8) . ?
C4 C5 1.422(7) . ?
C5 C6 1.431(8) . ?
C6 C7 1.415(7) . ?
C7 C8 1.392(8) . ?
C7 C14 1.511(7) . ?
C8 C9 1.379(7) . ?
C8 C15 1.510(8) . ?
C9 C17 1.487(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.502(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.510(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.520(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.393(8) . ?
C20 C25 1.373(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.388(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.397(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.388(8) . ?
C26 C31 1.377(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.375(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.376(9) . ?
C31 H31 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C20 P1 C19 99.0(2) . . ?
C20 P1 C26 100.6(3) . . ?
C26 P1 C19 103.7(2) . . ?
C1 N1 C4 108.0(4) . . ?
C1 N1 B1 125.5(4) . . ?
C4 N1 B1 126.4(4) . . ?
C6 N2 B1 126.1(4) . . ?
C9 N2 C6 107.8(4) . . ?
C9 N2 B1 125.9(4) . . ?
C5 N3 H3 111(3) . . ?
C5 N3 C18 121.9(4) . . ?
C18 N3 H3 119(3) . . ?
N1 C1 C2 108.6(4) . . ?
N1 C1 C10 122.9(5) . . ?
C2 C1 C10 128.5(5) . . ?
C1 C2 C11 125.6(5) . . ?
C3 C2 C1 108.0(5) . . ?
C3 C2 C11 126.4(5) . . ?
C2 C3 C4 106.0(5) . . ?
C2 C3 C13 125.7(5) . . ?
C4 C3 C13 128.3(5) . . ?
N1 C4 C3 109.4(4) . . ?
N1 C4 C5 119.6(4) . . ?
C3 C4 C5 131.0(5) . . ?
N3 C5 C4 120.8(5) . . ?
N3 C5 C6 119.7(5) . . ?
C4 C5 C6 119.5(5) . . ?
N2 C6 C5 120.0(4) . . ?
N2 C6 C7 108.2(4) . . ?
C7 C6 C5 131.1(5) . . ?
C6 C7 C14 127.5(5) . . ?
C8 C7 C6 106.8(4) . . ?
C8 C7 C14 125.2(5) . . ?
C7 C8 C15 125.6(5) . . ?
C9 C8 C7 107.8(5) . . ?
C9 C8 C15 126.7(5) . . ?
N2 C9 C8 109.4(5) . . ?
N2 C9 C17 123.2(5) . . ?
C8 C9 C17 127.3(5) . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 C11 H11A 109.1 . . ?
C2 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 C2 112.5(5) . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 H15A 109.2 . . ?
C8 C15 H15B 109.2 . . ?
C8 C15 C16 111.9(5) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
N3 C18 C19 110.6(4) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
P1 C19 H19A 109.2 . . ?
P1 C19 H19B 109.2 . . ?
C18 C19 P1 111.9(4) . . ?
C18 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 P1 116.0(4) . . ?
C25 C20 P1 124.7(4) . . ?
C25 C20 C21 119.2(5) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.5(6) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(6) . . ?
C23 C22 H22 120.2 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.8(5) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.8(6) . . ?
C25 C24 H24 120.6 . . ?
C20 C25 C24 121.1(5) . . ?
C20 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 P1 125.8(4) . . ?
C31 C26 P1 116.2(4) . . ?
C31 C26 C27 117.6(5) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C27 C28 H28 119.4 . . ?
C27 C28 C29 121.3(5) . . ?
C29 C28 H28 119.4 . . ?
C28 C29 H29 121.2 . . ?
C30 C29 C28 117.7(6) . . ?
C30 C29 H29 121.2 . . ?
C29 C30 H30 119.7 . . ?
C31 C30 C29 120.5(6) . . ?
C31 C30 H30 119.7 . . ?
C26 C31 H31 119.1 . . ?
C30 C31 C26 121.9(6) . . ?
C30 C31 H31 119.1 . . ?
F1 B1 N1 110.4(4) . . ?
F1 B1 N2 112.0(4) . . ?
F2 B1 F1 108.2(4) . . ?
F2 B1 N1 109.6(4) . . ?
F2 B1 N2 110.6(4) . . ?
N2 B1 N1 106.1(4) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C20 C21 C22 -177.5(4) . . . . ?
P1 C20 C25 C24 177.2(4) . . . . ?
P1 C26 C27 C28 -177.7(5) . . . . ?
P1 C26 C31 C30 179.8(7) . . . . ?
N1 C1 C2 C3 -3.2(6) . . . . ?
N1 C1 C2 C11 177.2(5) . . . . ?
N1 C4 C5 N3 -167.2(4) . . . . ?
N1 C4 C5 C6 13.0(7) . . . . ?
N2 C6 C7 C8 -1.6(5) . . . . ?
N2 C6 C7 C14 170.8(5) . . . . ?
N3 C5 C6 N2 168.8(4) . . . . ?
N3 C5 C6 C7 -22.5(8) . . . . ?
N3 C18 C19 P1 175.3(4) . . . . ?
C1 N1 C4 C3 -2.6(6) . . . . ?
C1 N1 C4 C5 175.2(4) . . . . ?
C1 N1 B1 F1 -64.7(6) . . . . ?
C1 N1 B1 F2 54.4(6) . . . . ?
C1 N1 B1 N2 173.8(4) . . . . ?
C1 C2 C3 C4 1.5(6) . . . . ?
C1 C2 C3 C13 179.3(5) . . . . ?
C1 C2 C11 C12 97.0(7) . . . . ?
C2 C3 C4 N1 0.6(6) . . . . ?
C2 C3 C4 C5 -176.8(5) . . . . ?
C3 C2 C11 C12 -82.6(7) . . . . ?
C3 C4 C5 N3 10.0(8) . . . . ?
C3 C4 C5 C6 -169.8(5) . . . . ?
C4 N1 C1 C2 3.5(6) . . . . ?
C4 N1 C1 C10 -174.6(5) . . . . ?
C4 N1 B1 F1 110.6(5) . . . . ?
C4 N1 B1 F2 -130.4(5) . . . . ?
C4 N1 B1 N2 -11.0(6) . . . . ?
C4 C5 C6 N2 -11.4(7) . . . . ?
C4 C5 C6 C7 157.4(5) . . . . ?
C5 N3 C18 C19 -100.1(6) . . . . ?
C5 C6 C7 C8 -171.4(5) . . . . ?
C5 C6 C7 C14 1.1(9) . . . . ?
C6 N2 C9 C8 -1.1(6) . . . . ?
C6 N2 C9 C17 -179.0(5) . . . . ?
C6 N2 B1 F1 -107.9(5) . . . . ?
C6 N2 B1 F2 131.4(5) . . . . ?
C6 N2 B1 N1 12.6(6) . . . . ?
C6 C7 C8 C9 1.0(6) . . . . ?
C6 C7 C8 C15 179.9(5) . . . . ?
C7 C8 C9 N2 0.0(6) . . . . ?
C7 C8 C9 C17 177.8(5) . . . . ?
C7 C8 C15 C16 71.6(7) . . . . ?
C9 N2 C6 C5 172.8(4) . . . . ?
C9 N2 C6 C7 1.7(5) . . . . ?
C9 N2 B1 F1 77.5(6) . . . . ?
C9 N2 B1 F2 -43.2(6) . . . . ?
C9 N2 B1 N1 -162.0(4) . . . . ?
C9 C8 C15 C16 -109.7(6) . . . . ?
C10 C1 C2 C3 174.8(5) . . . . ?
C10 C1 C2 C11 -4.8(9) . . . . ?
C11 C2 C3 C4 -178.9(5) . . . . ?
C11 C2 C3 C13 -1.1(9) . . . . ?
C13 C3 C4 N1 -177.1(5) . . . . ?
C13 C3 C4 C5 5.5(9) . . . . ?
C14 C7 C8 C9 -171.7(5) . . . . ?
C14 C7 C8 C15 7.2(8) . . . . ?
C15 C8 C9 N2 -178.8(5) . . . . ?
C15 C8 C9 C17 -1.1(9) . . . . ?
C18 N3 C5 C4 130.9(5) . . . . ?
C18 N3 C5 C6 -49.3(7) . . . . ?
C19 P1 C20 C21 110.5(4) . . . . ?
C19 P1 C20 C25 -66.8(5) . . . . ?
C19 P1 C26 C27 -2.2(6) . . . . ?
C19 P1 C26 C31 -175.6(5) . . . . ?
C20 P1 C19 C18 -174.0(4) . . . . ?
C20 P1 C26 C27 -104.2(5) . . . . ?
C20 P1 C26 C31 82.3(6) . . . . ?
C20 C21 C22 C23 -0.1(8) . . . . ?
C21 C20 C25 C24 -0.1(8) . . . . ?
C21 C22 C23 C24 0.4(9) . . . . ?
C22 C23 C24 C25 -0.6(8) . . . . ?
C23 C24 C25 C20 0.4(8) . . . . ?
C25 C20 C21 C22 -0.1(8) . . . . ?
C26 P1 C19 C18 82.6(4) . . . . ?
C26 P1 C20 C21 -143.7(4) . . . . ?
C26 P1 C20 C25 39.0(5) . . . . ?
C26 C27 C28 C29 0.7(9) . . . . ?
C27 C26 C31 C30 5.8(11) . . . . ?
C27 C28 C29 C30 1.5(11) . . . . ?
C28 C29 C30 C31 -0.1(13) . . . . ?
C29 C30 C31 C26 -3.6(14) . . . . ?
C31 C26 C27 C28 -4.3(9) . . . . ?
B1 N1 C1 C2 179.5(4) . . . . ?
B1 N1 C1 C10 1.4(8) . . . . ?
B1 N1 C4 C3 -178.5(4) . . . . ?
B1 N1 C4 C5 -0.7(7) . . . . ?
B1 N2 C6 C5 -2.7(7) . . . . ?
B1 N2 C6 C7 -173.7(4) . . . . ?
B1 N2 C9 C8 174.4(4) . . . . ?
B1 N2 C9 C17 -3.5(8) . . . . ?
_shelx_res_file
;
TITL n3522 in P2(1)/c
CELL 1.54178 8.4508 41.4961 8.07 90 94.122 90
ZERR 4 0.0004 0.0016 0.0003 0 0.0036 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H B F N P
UNIT 124 148 4 8 12 4
L.S. 4
PLAN 20
SIZE 0.021 0.098 0.15
TEMP -173.12
REM Solution 1 R1 0.162 Rweak 0.027, Alpha = 0.0553 in P2(1)/c
BOND $h
wpdb -2
MORE -1
CONF
fmap 2
acta
REM Z:/Charlotte/n3522/n3522af.hkl
WGHT 0.076400 7.746800
FVAR 0.15923
P1 6 0.383960 0.189084 0.487689 11.00000 0.03465 0.02095 =
0.02151 -0.00114 0.00002 0.00016
F1 4 1.073525 0.092080 0.484867 11.00000 0.02869 0.02580 =
0.03048 0.00359 -0.00578 -0.00658
F2 4 1.072850 0.046257 0.332867 11.00000 0.02846 0.02564 =
0.03857 0.00414 0.00827 0.00702
N1 5 0.847840 0.056107 0.491320 11.00000 0.01900 0.01588 =
0.02436 0.00159 -0.00106 0.00055
N2 5 0.888385 0.087853 0.239186 11.00000 0.02646 0.01754 =
0.02436 0.00069 0.00453 -0.00071
N3 5 0.476416 0.095703 0.346102 11.00000 0.02781 0.01760 =
0.02776 0.00335 0.00484 -0.00241
H3 2 0.420843 0.083868 0.405451 11.00000 0.00794
C1 1 0.875008 0.036352 0.626312 11.00000 0.02489 0.01994 =
0.02399 -0.00031 0.00272 -0.00364
C2 1 0.727951 0.028322 0.687586 11.00000 0.02625 0.02549 =
0.02950 -0.00125 0.00242 -0.00586
C3 1 0.609221 0.044950 0.593113 11.00000 0.02302 0.02425 =
0.02856 -0.00067 -0.00075 -0.00324
C4 1 0.687296 0.062288 0.472067 11.00000 0.02032 0.01875 =
0.02092 -0.00165 0.00378 -0.00512
C5 1 0.627973 0.084341 0.347762 11.00000 0.01650 0.01671 =
0.03342 -0.00116 -0.00353 -0.00252
C6 1 0.728621 0.094633 0.222663 11.00000 0.02669 0.01724 =
0.01797 -0.00118 0.00144 -0.00512
C7 1 0.692060 0.107279 0.061580 11.00000 0.01934 0.01762 =
0.02847 -0.00526 -0.00098 -0.00429
C8 1 0.833973 0.108726 -0.015623 11.00000 0.03180 0.01950 =
0.02444 -0.00396 0.00304 -0.00102
C9 1 0.952313 0.096825 0.094204 11.00000 0.03174 0.01958 =
0.02058 -0.00010 -0.00063 0.00276
C10 1 1.036444 0.026955 0.692870 11.00000 0.02732 0.02655 =
0.02734 0.00566 0.00057 -0.00291
AFIX 137
H10A 2 1.086743 0.013820 0.610489 11.00000 -1.50000
H10B 2 1.029282 0.014470 0.795140 11.00000 -1.50000
H10C 2 1.100059 0.046362 0.716993 11.00000 -1.50000
AFIX 0
C11 1 0.704416 0.005770 0.831515 11.00000 0.02439 0.02818 =
0.03744 0.00482 0.00207 0.00141
AFIX 23
H11A 2 0.607149 -0.007126 0.806001 11.00000 -1.20000
H11B 2 0.795266 -0.009305 0.844394 11.00000 -1.20000
AFIX 0
C12 1 0.690274 0.023446 0.992248 11.00000 0.03475 0.03116 =
0.04163 0.00754 0.00192 -0.00445
AFIX 137
H12A 2 0.593734 0.036606 0.984337 11.00000 -1.50000
H12B 2 0.782956 0.037399 1.014334 11.00000 -1.50000
H12C 2 0.684906 0.007862 1.082919 11.00000 -1.50000
AFIX 0
C13 1 0.435300 0.043106 0.615050 11.00000 0.02683 0.03450 =
0.03198 0.01133 0.00457 -0.00011
AFIX 137
H13A 2 0.399071 0.063650 0.658751 11.00000 -1.50000
H13B 2 0.414941 0.025767 0.693177 11.00000 -1.50000
H13C 2 0.377874 0.038692 0.507605 11.00000 -1.50000
AFIX 0
C14 1 0.529620 0.113895 -0.022076 11.00000 0.03787 0.02712 =
0.02761 -0.00455 0.00380 -0.00457
AFIX 137
H14A 2 0.450292 0.101031 0.031172 11.00000 -1.50000
H14B 2 0.528601 0.108108 -0.139884 11.00000 -1.50000
H14C 2 0.504594 0.136836 -0.011783 11.00000 -1.50000
AFIX 0
C15 1 0.852539 0.120653 -0.189942 11.00000 0.02861 0.03771 =
0.02315 0.00167 0.00130 0.00259
AFIX 23
H15A 2 0.772630 0.110008 -0.267284 11.00000 -1.20000
H15B 2 0.959021 0.114641 -0.223454 11.00000 -1.20000
AFIX 0
C16 1 0.832561 0.156734 -0.203458 11.00000 0.04599 0.04060 =
0.02822 0.01081 0.00920 -0.00025
AFIX 137
H16A 2 0.851449 0.163663 -0.316440 11.00000 -1.50000
H16B 2 0.908805 0.167342 -0.124031 11.00000 -1.50000
H16C 2 0.724461 0.162617 -0.178676 11.00000 -1.50000
AFIX 0
C17 1 1.122847 0.092605 0.065021 11.00000 0.02272 0.03776 =
0.02992 0.00071 -0.00348 -0.00103
AFIX 137
H17A 2 1.183319 0.088383 0.170994 11.00000 -1.50000
H17B 2 1.162804 0.112260 0.015204 11.00000 -1.50000
H17C 2 1.134790 0.074391 -0.010366 11.00000 -1.50000
AFIX 0
C18 1 0.439914 0.130485 0.330612 11.00000 0.02706 0.02445 =
0.02822 -0.00063 0.00441 0.00406
AFIX 23
H18A 2 0.343436 0.133532 0.255162 11.00000 -1.20000
H18B 2 0.528837 0.141737 0.281845 11.00000 -1.20000
AFIX 0
C19 1 0.413649 0.144951 0.499489 11.00000 0.02904 0.02372 =
0.02782 -0.00006 -0.00078 0.00411
AFIX 23
H19A 2 0.506602 0.140171 0.577335 11.00000 -1.20000
H19B 2 0.319414 0.134816 0.543838 11.00000 -1.20000
AFIX 0
C20 1 0.379379 0.197781 0.710419 11.00000 0.04052 0.01822 =
0.02079 0.00103 -0.00023 0.00626
C21 1 0.508819 0.214734 0.782793 11.00000 0.03604 0.02133 =
0.03372 0.00058 -0.00175 0.00257
AFIX 43
H21 2 0.590274 0.221759 0.716019 11.00000 -1.20000
AFIX 0
C22 1 0.519660 0.221437 0.951664 11.00000 0.04632 0.02644 =
0.02576 -0.00260 -0.00974 0.00199
AFIX 43
H22 2 0.608240 0.232973 1.000509 11.00000 -1.20000
AFIX 0
C23 1 0.401200 0.211262 1.048084 11.00000 0.05736 0.02573 =
0.02128 -0.00383 -0.00292 0.00383
AFIX 43
H23 2 0.408256 0.215984 1.163566 11.00000 -1.20000
AFIX 0
C24 1 0.271686 0.194196 0.978561 11.00000 0.05283 0.02454 =
0.02739 0.00443 0.00818 0.00793
AFIX 43
H24 2 0.190692 0.187045 1.045604 11.00000 -1.20000
AFIX 0
C25 1 0.262496 0.187718 0.808295 11.00000 0.03552 0.02174 =
0.03225 -0.00185 0.00335 0.00176
AFIX 43
H25 2 0.173980 0.176166 0.759415 11.00000 -1.20000
AFIX 0
C26 1 0.172340 0.193362 0.419713 11.00000 0.03772 0.02097 =
0.02755 -0.00018 0.00140 -0.00061
C27 1 0.067279 0.168255 0.381984 11.00000 0.03165 0.02143 =
0.03600 0.00394 0.00165 0.00322
AFIX 43
H27 2 0.102794 0.146615 0.394637 11.00000 -1.20000
AFIX 0
C28 1 -0.087575 0.174315 0.326516 11.00000 0.03763 0.02717 =
0.04001 -0.00348 0.00380 -0.00702
AFIX 43
H28 2 -0.157671 0.156754 0.302696 11.00000 -1.20000
AFIX 0
C29 1 -0.143497 0.205661 0.304636 11.00000 0.03865 0.04535 =
0.05989 0.00450 -0.01909 0.00178
AFIX 43
H29 2 -0.251112 0.209821 0.268850 11.00000 -1.20000
AFIX 0
C30 1 -0.036438 0.230673 0.336958 11.00000 0.04937 0.02511 =
0.10441 -0.00154 -0.02586 -0.00021
AFIX 43
H30 2 -0.070827 0.252363 0.323018 11.00000 -1.20000
AFIX 0
C31 1 0.118984 0.224281 0.388992 11.00000 0.04409 0.02440 =
0.07692 -0.00319 -0.02358 -0.00111
AFIX 43
H31 2 0.191542 0.241698 0.404152 11.00000 -1.20000
AFIX 0
B1 3 0.977248 0.070730 0.387580 11.00000 0.02893 0.01179 =
0.02174 0.00069 -0.00055 -0.00351
HKLF 4
REM n3522 in P2(1)/c
REM R1 = 0.0838 for 3111 Fo > 4sig(Fo) and 0.1133 for all 4343 data
REM 353 parameters refined using 0 restraints
END
WGHT 0.0769 7.7097
REM Highest difference peak 0.781, deepest hole -0.398, 1-sigma level 0.075
Q1 1 0.2724 0.1864 0.4785 11.00000 0.05 0.78
Q2 1 0.1230 0.1933 0.9844 11.00000 0.05 0.38
Q3 1 0.4041 0.1663 0.4811 11.00000 0.05 0.32
Q4 1 0.5683 0.0641 0.4559 11.00000 0.05 0.32
Q5 1 0.3635 0.0981 0.3488 11.00000 0.05 0.32
Q6 1 0.2735 0.2007 0.7010 11.00000 0.05 0.32
Q7 1 0.2749 0.2151 1.0379 11.00000 0.05 0.32
Q8 1 1.2164 0.0969 0.3622 11.00000 0.05 0.31
Q9 1 0.5455 0.0567 0.2762 11.00000 0.05 0.31
Q10 1 0.3256 0.1253 0.3307 11.00000 0.05 0.31
Q11 1 0.7545 0.0516 0.4697 11.00000 0.05 0.31
Q12 1 0.9635 0.0944 0.4766 11.00000 0.05 0.30
Q13 1 0.7007 -0.0207 0.8624 11.00000 0.05 0.30
Q14 1 0.4032 0.2135 0.7728 11.00000 0.05 0.30
Q15 1 0.6526 0.0454 0.7170 11.00000 0.05 0.30
Q16 1 0.6068 0.1055 0.0391 11.00000 0.05 0.30
Q17 1 0.7385 0.1054 -0.0230 11.00000 0.05 0.29
Q18 1 0.2343 0.0400 0.6010 11.00000 0.05 0.29
Q19 1 0.6330 0.0897 0.2183 11.00000 0.05 0.28
Q20 1 0.5803 0.1021 0.4388 11.00000 0.05 0.28
;
_shelx_res_checksum 67121
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;
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-2 0 0 127.42 2.11
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-4 0 0 177.14 3.58
-4 0 0 216.31 2.80
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-5 0 0 57.56 2.34
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-4 5 0 1.74 1.06
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-6 7 0 55.95 2.31
-6 7 0 63.05 2.71
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1 14 0 105.28 2.85
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0 15 0 0.21 1.04
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1 15 0 36.95 2.20
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2 15 0 43.73 2.43
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-4 -11 -7 -0.81 1.26
-4 -11 -7 0.14 1.11
-6 -12 7 0.38 1.27
2 12 -7 3.76 1.45
-2 12 7 4.22 1.26
1 12 -7 0.67 1.39
-1 12 7 1.45 1.20
0 12 -7 4.84 1.51
0 12 7 3.80 1.33
-1 12 -7 11.58 2.10
-1 -12 -7 9.06 1.89
-1 -12 -7 6.67 1.55
1 12 7 10.74 1.91
-2 12 -7 9.02 1.66
-2 -12 -7 8.38 1.93
-2 -12 -7 6.20 1.31
-3 12 -7 5.44 1.50
-3 -12 -7 6.35 1.49
-3 -12 -7 5.42 1.28
-4 -12 -7 2.26 1.37
-4 -12 -7 2.14 1.17
-6 -13 7 3.50 1.31
-5 -13 7 0.80 1.51
2 13 -7 2.69 1.46
-2 13 7 1.22 1.15
-2 -13 7 2.46 1.47
1 13 -7 -0.03 1.36
-1 13 7 0.75 1.18
0 13 -7 5.06 1.58
0 13 7 3.97 1.34
-1 13 -7 2.17 1.49
-1 -13 -7 1.78 1.31
-1 -13 -7 1.81 1.08
1 13 7 0.31 1.28
-2 13 -7 4.03 1.50
-2 -13 -7 5.01 1.43
-2 -13 -7 5.32 1.28
-3 13 -7 20.65 2.02
-3 -13 -7 18.17 2.04
-3 -13 -7 15.56 1.81
-4 -13 -7 6.85 1.50
-4 -13 -7 5.02 1.22
-6 -14 7 2.57 1.24
-5 -14 7 2.16 1.52
3 14 -7 8.41 1.98
2 14 -7 4.79 1.56
-2 14 7 4.88 1.26
1 14 -7 0.52 1.38
-1 14 7 0.35 1.19
0 14 -7 20.65 2.18
0 14 7 19.78 1.96
-1 14 -7 0.75 1.45
-1 -14 -7 0.38 1.30
-1 -14 -7 0.44 1.04
1 14 7 0.66 1.31
-2 14 -7 20.88 2.20
-2 -14 -7 19.05 2.12
-2 -14 -7 15.21 1.75
-3 -14 -7 1.59 1.29
-3 -14 -7 0.25 1.07
-4 -14 -7 0.80 1.31
-4 -14 -7 1.87 1.14
-6 -15 7 2.02 1.21
-5 -15 7 14.62 1.99
3 15 -7 0.90 1.37
2 15 -7 2.12 1.42
-2 15 7 2.30 1.18
-2 -15 7 -0.27 1.41
1 15 -7 2.86 1.46
-1 15 7 1.14 1.24
0 15 -7 6.32 1.62
0 -15 -7 5.24 1.25
0 15 7 7.62 1.79
-1 15 -7 14.22 2.14
-1 -15 -7 12.66 2.01
-1 -15 -7 10.85 1.62
1 15 7 14.04 1.94
-2 15 -7 2.58 1.53
-2 -15 -7 1.14 1.32
-2 -15 -7 1.53 1.14
-3 -15 -7 11.51 2.01
-3 -15 -7 9.00 1.69
-4 -15 -7 0.25 1.33
-4 -15 -7 0.14 1.07
-6 -16 7 0.21 1.15
-5 -16 7 -0.80 1.36
3 16 -7 8.18 1.98
2 16 -7 0.08 1.34
-2 16 7 1.29 1.14
1 16 -7 2.04 1.44
-1 16 7 2.28 1.22
0 16 -7 4.87 1.61
0 -16 -7 3.04 1.11
0 16 7 2.72 1.35
-1 16 -7 3.95 1.56
-1 -16 -7 2.93 1.38
-1 -16 -7 2.75 1.15
1 16 7 2.81 1.41
-2 16 -7 0.72 1.37
-2 -16 -7 0.02 1.36
-2 -16 -7 0.55 1.11
-3 16 -7 2.43 1.28
-3 -16 -7 2.43 1.39
-3 -16 -7 1.65 1.14
-4 -16 -7 1.72 1.35
-4 -16 -7 2.50 1.15
-5 -17 7 4.42 1.50
3 17 -7 5.54 1.53
2 17 -7 3.24 1.44
1 17 -7 4.08 1.50
-1 17 7 5.54 1.33
0 17 -7 1.05 1.40
0 -17 -7 1.31 1.05
0 17 7 0.96 1.32
-1 17 -7 1.22 1.40
-1 -17 -7 1.12 1.36
-1 -17 -7 -0.48 1.01
1 17 7 1.38 1.35
-2 17 -7 8.09 1.56
-2 -17 -7 8.93 2.03
-2 -17 -7 6.35 1.28
-3 -17 -7 1.74 1.32
-3 -17 -7 2.16 1.15
3 -17 7 2.97 1.43
-4 -17 -7 5.56 1.45
-4 -17 -7 5.09 1.17
-5 -18 7 0.08 1.30
4 18 -7 0.58 1.27
3 18 -7 2.76 1.50
2 18 -7 8.64 1.69
1 18 -7 0.03 1.43
-1 18 7 0.27 1.21
0 18 -7 8.91 2.09
0 -18 -7 7.62 1.29
0 18 7 8.21 1.84
-1 18 -7 3.19 1.49
-1 -18 -7 3.60 1.45
-1 -18 -7 3.04 1.19
1 18 7 3.92 1.43
-2 18 -7 1.83 1.39
-2 -18 -7 1.39 1.38
-2 -18 -7 1.51 1.12
2 -18 7 2.13 1.38
-3 -18 -7 6.08 1.46
-3 -18 -7 5.41 1.27
-4 -18 -7 1.30 1.28
-4 -18 -7 0.74 1.05
-5 -19 7 15.80 1.80
4 19 -7 7.09 1.55
3 19 -7 -0.73 1.36
2 19 -7 4.75 1.53
1 19 -7 2.07 1.49
-1 19 7 2.71 1.28
0 19 -7 2.67 1.49
0 -19 -7 1.80 1.06
0 19 7 1.09 1.27
-1 19 -7 3.26 1.50
-1 -19 -7 3.11 1.42
-1 -19 -7 2.85 1.17
1 19 7 2.51 1.39
-2 19 -7 3.42 1.40
-2 -19 -7 3.41 1.45
-2 -19 -7 3.08 1.17
-3 -19 -7 1.70 1.31
-3 -19 -7 1.89 1.11
-4 -19 -7 9.40 1.81
-4 -19 -7 7.05 1.48
-5 -20 7 2.70 1.27
4 20 -7 4.05 1.41
3 20 -7 2.35 1.43
2 20 -7 1.96 1.46
1 20 -7 0.21 1.49
-1 20 7 -0.08 1.16
0 20 -7 10.62 2.08
0 -20 -7 6.88 1.53
0 20 7 8.63 1.93
-1 20 -7 6.68 1.57
-1 -20 -7 5.52 1.51
-1 -20 -7 4.16 1.21
1 20 7 6.59 1.50
-2 20 -7 32.55 2.18
-2 -20 -7 30.82 2.33
-2 -20 -7 26.92 1.88
-3 -20 -7 9.91 1.90
-3 -20 -7 7.35 1.58
-4 -20 -7 0.07 1.25
-4 -20 -7 2.26 1.04
5 21 -7 1.73 1.16
-5 -21 7 1.35 1.16
4 21 -7 17.49 1.93
3 21 -7 3.57 1.47
2 21 -7 0.78 1.39
1 21 -7 0.38 1.39
-1 21 7 1.32 1.22
0 21 -7 28.68 2.23
0 -21 -7 22.71 1.77
0 21 7 32.30 2.22
-1 21 -7 -0.39 1.40
-1 -21 -7 1.16 1.37
-1 -21 -7 -0.34 1.04
1 21 7 -2.16 1.24
-2 21 -7 4.06 1.33
-2 -21 -7 4.06 1.47
-2 -21 -7 4.15 1.21
-3 -21 -7 26.98 2.10
-3 -21 -7 23.06 1.74
-4 -21 -7 1.55 1.21
-4 -21 -7 0.57 0.94
5 22 -7 0.73 1.10
4 22 -7 3.31 1.32
-4 -22 7 3.48 1.39
3 22 -7 13.95 2.05
2 22 -7 0.26 1.39
1 22 -7 0.27 1.46
-1 22 7 1.32 1.17
0 22 -7 0.41 1.45
0 -22 -7 -0.30 1.01
0 22 7 -0.25 1.21
-1 22 -7 -0.09 1.31
-1 -22 -7 0.21 1.31
-1 -22 -7 0.23 1.05
1 22 7 0.49 1.34
-2 22 -7 7.13 1.71
-2 -22 -7 9.30 1.61
-2 -22 -7 6.79 1.57
-3 -22 -7 7.79 1.57
-3 -22 -7 4.65 1.19
-4 -22 -7 -0.08 1.15
-4 -22 -7 -0.66 0.87
4 23 -7 1.04 1.26
3 23 -7 6.88 1.55
2 23 -7 1.22 1.44
1 23 -7 -1.06 1.31
-1 23 7 -0.94 1.14
0 23 -7 18.05 2.12
0 -23 -7 11.52 1.62
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-1 23 -7 6.55 1.45
-1 -23 -7 7.28 1.51
-1 -23 -7 6.90 1.28
1 23 7 7.97 1.89
-2 -23 -7 3.05 1.38
-2 -23 -7 2.32 1.13
-3 -23 -7 5.40 1.45
-3 -23 -7 3.93 1.14
-4 -23 -7 1.86 1.16
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4 24 -7 0.54 1.16
3 24 -7 2.06 1.38
2 24 -7 5.34 1.49
1 24 -7 3.50 1.51
-1 24 7 2.43 1.27
0 24 -7 15.73 2.04
0 -24 -7 11.27 1.64
0 24 7 14.94 1.92
-1 24 -7 1.43 1.28
-1 -24 -7 0.48 1.33
-1 -24 -7 0.73 1.05
1 24 7 0.86 1.29
-2 -24 -7 0.82 1.32
-2 -24 -7 1.62 1.06
-3 -24 -7 7.66 1.50
-3 -24 -7 6.09 1.41
4 25 -7 1.97 1.17
3 25 -7 -0.51 1.24
2 25 -7 4.30 1.41
1 25 -7 3.19 1.50
-1 25 7 1.45 1.24
0 25 -7 11.58 1.95
0 -25 -7 9.50 1.61
0 25 7 12.29 1.89
-1 25 -7 7.24 1.76
-1 -25 -7 7.42 1.50
-1 -25 -7 6.44 1.24
1 25 7 7.78 1.86
-2 -25 -7 0.36 1.29
-2 -25 -7 -0.09 1.02
-3 -25 -7 0.70 1.24
-3 -25 -7 0.86 0.97
4 26 -7 12.90 1.62
3 26 -7 0.16 1.20
2 26 -7 21.48 1.98
1 26 -7 2.20 1.38
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0 26 -7 5.86 1.46
0 -26 -7 3.77 1.13
0 26 7 5.03 1.36
-1 26 -7 4.73 1.28
-1 -26 -7 4.72 1.39
-1 -26 -7 5.00 1.17
1 26 7 6.04 1.42
-2 -26 -7 -0.38 1.22
-2 -26 -7 -0.04 0.98
-3 -26 -7 0.48 1.17
-3 -26 -7 0.51 0.91
3 27 -7 5.68 1.32
2 27 -7 0.94 1.29
1 27 -7 10.99 1.81
0 27 -7 0.95 1.25
0 -27 -7 0.13 0.99
0 27 7 -0.60 1.21
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-1 -27 -7 7.89 1.50
1 27 7 11.23 1.85
-2 -27 -7 4.22 1.33
-2 -27 -7 4.06 1.07
-3 -27 -7 5.52 1.09
3 28 -7 16.73 1.63
2 28 -7 1.84 1.23
1 28 -7 5.37 1.39
0 28 -7 -0.23 1.20
0 -28 -7 0.30 0.97
-1 -28 -7 0.16 1.22
-1 -28 -7 0.04 0.95
1 28 7 0.74 1.22
-2 -28 -7 12.37 1.81
-2 -28 -7 10.90 1.45
3 29 -7 10.44 1.50
2 29 -7 2.26 1.21
1 29 -7 1.78 1.24
0 29 -7 10.33 1.62
0 -29 -7 8.35 1.38
0 29 7 11.42 1.78
-1 -29 -7 -0.45 0.91
-2 -29 -7 2.29 1.21
-2 -29 -7 1.64 0.92
2 30 -7 1.94 1.12
1 30 -7 4.52 1.22
0 30 -7 5.84 1.18
0 -30 -7 5.05 1.06
-1 -30 -7 1.04 0.92
2 31 -7 5.00 1.11
1 31 -7 0.74 1.08
0 31 -7 3.32 1.05
0 31 7 2.32 1.12
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0 0 -8 5.69 1.63
-1 0 -8 8.15 1.70
-2 0 -8 1.84 1.43
-3 0 -8 7.07 1.53
-5 1 8 1.34 1.11
-5 -1 8 1.21 1.14
1 1 -8 0.72 1.43
0 1 -8 25.75 2.30
0 -1 -8 25.45 2.22
-1 1 -8 13.46 2.09
-1 -1 -8 14.74 2.15
-2 1 -8 7.82 1.58
-2 -1 -8 8.31 1.58
-3 1 -8 1.73 1.36
-5 2 8 6.47 1.24
-5 -2 8 7.23 1.59
1 2 -8 12.53 2.09
0 2 -8 0.58 1.48
0 -2 -8 2.33 1.42
-1 2 -8 5.45 1.62
-1 -2 -8 3.93 1.51
-2 2 -8 15.60 2.08
-2 -2 -8 13.82 2.09
-5 3 8 0.27 1.07
-5 -3 8 1.66 1.18
1 3 -8 2.00 1.44
0 3 -8 44.00 2.49
0 -3 -8 40.23 2.41
-1 3 -8 2.31 1.50
-1 -3 -8 0.92 1.43
-2 3 -8 12.24 2.10
-2 -3 -8 9.52 2.07
-3 3 -8 -0.06 1.27
-3 -3 -8 0.78 1.35
-5 4 8 1.08 1.06
-5 -4 8 1.14 1.17
1 4 -8 1.21 1.47
0 4 -8 2.78 1.52
0 -4 -8 2.92 1.46
-1 4 -8 0.26 1.44
-1 -4 -8 0.71 1.46
-2 4 -8 0.37 1.39
-2 -4 -8 0.92 1.37
-3 -4 -8 2.18 1.38
-5 -5 8 1.41 1.19
1 5 -8 3.81 1.55
0 5 -8 6.92 1.62
0 -5 -8 6.81 1.52
-1 5 -8 16.00 2.19
-1 -5 -8 16.26 2.22
-2 5 -8 2.30 1.36
-2 -5 -8 0.77 1.41
-3 5 -8 10.61 1.89
-3 -5 -8 10.86 1.94
-5 -6 8 6.16 1.34
1 6 -8 35.09 2.38
0 6 -8 2.92 1.55
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-1 6 -8 2.26 1.46
-1 -6 -8 3.13 1.49
-2 6 -8 2.59 1.48
-2 -6 -8 3.59 1.51
-3 6 -8 5.28 1.38
-3 -6 -8 4.33 1.44
-5 -7 8 2.87 1.22
1 7 -8 0.10 1.40
0 7 -8 0.70 1.43
0 -7 -8 1.56 1.43
-1 7 -8 3.33 1.49
-1 -7 -8 3.21 1.53
-2 7 -8 2.83 1.43
-2 -7 -8 3.61 1.48
-3 -7 -8 3.27 1.38
-5 -8 8 0.13 1.19
2 8 -8 2.99 1.45
1 8 -8 4.88 1.60
0 8 -8 15.16 2.20
0 -8 -8 15.68 2.07
-1 8 -8 0.24 1.35
-1 -8 -8 0.49 1.43
-2 8 -8 1.89 1.37
-2 -8 -8 0.66 1.40
-3 -8 -8 8.12 1.49
-5 -9 8 -0.71 1.13
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1 9 -8 0.84 1.37
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-1 9 -8 1.39 1.41
-1 -9 -8 -0.90 1.38
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-2 -9 -8 -0.06 1.39
-2 -9 -8 -0.69 0.94
-3 -9 -8 0.99 1.28
-5 -10 8 4.52 1.27
2 10 -8 17.74 2.15
1 10 -8 0.38 1.45
0 10 -8 0.35 1.47
-1 10 -8 0.81 1.48
-1 -10 -8 0.86 1.47
-2 10 -8 3.75 1.43
-2 -10 -8 2.99 1.45
-2 -10 -8 2.88 1.07
-5 -11 8 -0.56 1.14
2 11 -8 0.60 1.39
1 11 -8 1.18 1.38
0 11 -8 7.97 1.68
-1 11 -8 2.33 1.46
-1 -11 -8 2.20 1.44
-2 11 -8 3.55 1.38
-2 -11 -8 1.79 1.43
-2 -11 -8 2.33 1.02
-3 -11 -8 3.27 1.36
-5 -12 8 2.34 1.19
2 12 -8 2.39 1.39
1 12 -8 7.03 1.62
0 12 -8 6.57 1.59
-1 12 -8 0.90 1.38
-1 -12 -8 -0.08 1.37
-2 -12 -8 4.38 1.55
-2 -12 -8 2.76 1.04
-3 -12 -8 1.48 1.26
3 13 -8 1.01 1.28
2 13 -8 0.73 1.34
1 13 -8 2.60 1.49
0 13 -8 10.45 2.09
-1 13 -8 1.23 1.40
-2 -13 -8 3.19 1.38
-2 -13 -8 3.93 1.06
-3 -13 -8 0.60 1.23
3 14 -8 3.99 1.36
2 14 -8 7.80 1.95
1 14 -8 10.70 1.96
0 14 -8 2.25 1.39
-1 14 -8 3.29 1.50
-1 -14 -8 3.40 1.44
-2 14 -8 3.17 1.34
-2 -14 -8 2.13 1.38
-2 -14 -8 1.73 0.98
-3 -14 -8 -0.56 0.92
3 15 -8 2.60 1.33
2 15 -8 2.51 1.40
1 15 -8 0.29 1.37
0 15 -8 8.98 1.58
-1 15 -8 8.27 1.88
-1 -15 -8 7.31 1.58
-2 -15 -8 12.67 2.04
-2 -15 -8 10.46 1.46
-3 -15 -8 6.00 1.37
-3 -15 -8 3.01 0.99
3 16 -8 -0.32 1.20
2 16 -8 12.36 1.99
1 16 -8 10.25 1.95
0 16 -8 -0.13 1.33
-1 16 -8 2.74 1.40
-1 -16 -8 2.75 1.42
-2 -16 -8 4.47 1.44
-2 -16 -8 3.85 1.03
-3 -16 -8 9.03 1.70
-3 -16 -8 8.31 1.33
4 17 -8 5.48 1.23
3 17 -8 6.75 1.36
2 17 -8 6.23 1.48
1 17 -8 6.49 1.51
0 17 -8 -0.26 1.35
-1 17 -8 11.74 1.85
-1 -17 -8 11.09 1.96
-2 -17 -8 -0.05 1.27
-2 -17 -8 1.14 0.93
-3 -17 -8 1.95 1.17
4 18 -8 3.60 1.12
3 18 -8 1.31 1.22
2 18 -8 5.51 1.41
1 18 -8 23.18 2.07
0 18 -8 2.80 1.37
-1 18 -8 -0.28 1.27
-1 -18 -8 0.35 1.26
-2 -18 -8 1.85 1.29
-2 -18 -8 3.29 0.96
3 19 -8 4.92 1.25
2 19 -8 5.07 1.33
1 19 -8 0.65 1.27
0 19 -8 18.92 1.94
-1 19 -8 -0.03 1.24
-1 -19 -8 1.94 1.34
-2 -19 -8 24.56 1.49
3 20 -8 6.59 1.59
2 20 -8 1.88 1.20
1 20 -8 1.03 1.28
0 20 -8 2.26 1.29
-1 20 -8 0.32 1.16
-1 -20 -8 -0.56 1.22
-1 -20 -8 -0.42 0.85
-2 -20 -8 1.41 0.90
3 21 -8 1.04 1.05
2 21 -8 2.74 1.22
1 21 -8 0.30 1.19
0 21 -8 1.33 1.22
-1 21 -8 -0.09 1.09
-1 -21 -8 -0.16 0.83
2 22 -8 0.60 1.19
1 22 -8 0.09 1.18
0 22 -8 5.02 1.27
-1 22 -8 -0.51 1.06
2 23 -8 10.01 1.59
1 23 -8 -0.09 1.16
0 23 -8 21.50 1.76
-1 -23 -8 0.57 1.15
1 24 -8 6.76 1.58
0 24 -8 7.38 1.59
-2 -1 -9 0.27 1.07
0 4 -9 0.46 1.32
-1 6 -9 11.50 1.73
0 7 -9 4.69 1.33
-1 7 -9 0.43 1.15
1 8 -9 0.72 1.20
0 8 -9 -0.66 1.16
-1 8 -9 5.31 1.28
0 9 -9 3.62 1.25
-1 9 -9 4.28 1.19
2 10 -9 -1.15 1.02
1 10 -9 1.29 1.16
0 10 -9 5.14 1.29
-1 10 -9 11.62 1.54
0 11 -9 0.27 1.14
1 12 -9 1.44 1.13
0 12 -9 0.56 1.08
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 54416
#===end
data_X1
_audit_creation_date 2014-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number 2013-4
_publ_contact_author_address ?
_publ_contact_author_email ?
_publ_contact_author_name ''
_publ_contact_author_phone ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety
'C154 H142 B2 F12 N8 P4 Rh2 S4 Zn, 2(C F3 O3 S)'
_chemical_formula_sum 'C156 H142 B2 F18 N8 O6 P4 Rh2 S6 Zn'
_chemical_formula_weight 3175.82
_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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Zn' 'Zn' -1.5491 0.6778
'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 'triclinic'
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 15.6349(9)
_cell_length_b 18.4356(12)
_cell_length_c 21.7530(15)
_cell_angle_alpha 107.517(4)
_cell_angle_beta 110.288(4)
_cell_angle_gamma 96.416(4)
_cell_volume 5442.2(6)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 6139
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 54.756
_cell_measurement_theta_min 3.933
_shelx_estimated_absorpt_T_max 0.942
_shelx_estimated_absorpt_T_min 0.699
_exptl_absorpt_coefficient_mu 2.620
_exptl_absorpt_correction_T_max 0.7507
_exptl_absorpt_correction_T_min 0.5457
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0799 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7269.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour pink
_exptl_crystal_colour_primary pink
_exptl_crystal_density_diffrn 0.969
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1630
_exptl_crystal_size_max 0.147
_exptl_crystal_size_mid 0.063
_exptl_crystal_size_min 0.023
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0533
_diffrn_reflns_av_unetI/netI 0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.542
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 14784
_diffrn_reflns_point_group_measured_fraction_full 0.542
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 50.849
_diffrn_reflns_theta_min 2.590
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.542
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'MX optics'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source microsource
_diffrn_standards_number .
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5820
_reflns_number_total 10661
_reflns_special_details
;
Data were apparently pre-merged, so _diffrn_reflns_number
etc. will have to be added later.
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 'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max 2.863
_refine_diff_density_min -1.700
_refine_diff_density_rms 0.162
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.333
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 871
_refine_ls_number_reflns 10661
_refine_ls_number_restraints 960
_refine_ls_R_factor_all 0.1940
_refine_ls_R_factor_gt 0.1434
_refine_ls_restrained_S_all 1.287
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3731
_refine_ls_wR_factor_ref 0.4064
_refine_special_details
'The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied globally. (Acta Cryst. A68 (2012) 448-451). The disordered triflate was refined as a rigid group with a group anistropic displacement parameter.'
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C2-C1 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C6-C1
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S3) = Uanis(O1) = Uanis(O4) = Uanis(O5) = Uanis(C1A) = Uanis(F7) =
Uanis(F8) = Uanis(F9)
Uanis(S3) = Uanis(O1) = Uanis(O4) = Uanis(O5) = Uanis(C1A) = Uanis(F7) =
Uanis(F8) = Uanis(F9) = Uanis(C6A) = Uanis(S3A) = Uanis(F7A) = Uanis(F8A) =
Uanis(F9A) = Uanis(O1A) = Uanis(O4A) = Uanis(O5A)
4. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Sof(C6A)=Sof(S3A)=Sof(O1A)=Sof(O4A)=Sof(O5A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=1-
FVAR(1)
Sof(S3)=Sof(O1)=Sof(O4)=Sof(O5)=Sof(C1A)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
6.a Free rotating group:
S3(O1,O4,O5,C1A,F7,F8,F9), C6A(S3A,O1A,O4A,O5A,F7A,F8A,F9A)
6.b Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C14(H14A,H14B), C31(H31A,H31B), C35(H35A,H35B), C50(H50A,
H50B), C51(H51A,H51B), C52(H52A,H52B)
6.c Me refined with riding coordinates:
C36(H36A,H36B,H36C)
6.d Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
C12(H12), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46),
C47(H47), C48(H48), C49(H49), C54(H54), C55(H55), C57(H57), C58(H58),
C61(H61), C62(H62), C65(H65), C66(H66), C71(H71), C73(H73)
6.e Idealised Me refined as rotating group:
C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
H34C), C37(H37A,H37B,H37C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,
H77B,H77C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_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
Rh1 Rh 0.66307(9) 0.68833(7) 0.04859(7) 0.0513(5) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.5000 0.5000 0.0780(12) Uani 1 2 d S T P . .
S1 S 0.5020(3) 0.6462(2) -0.0201(2) 0.0531(11) Uani 1 1 d . . . . .
S2 S 0.6342(3) 0.6846(2) 0.1460(2) 0.0552(12) Uani 1 1 d . . . . .
P1 P 0.6783(3) 0.6804(2) -0.0519(2) 0.0477(11) Uani 1 1 d . . . . .
P2 P 0.8156(3) 0.7237(2) 0.1212(2) 0.0537(12) Uani 1 1 d . . . . .
F1 F 0.5378(8) 0.8246(6) 0.0250(6) 0.082(3) Uani 1 1 d . . . . .
F2 F 0.4594(9) 0.9166(6) 0.0993(7) 0.104(4) Uani 1 1 d . . . . .
F3 F 0.2869(8) 0.6969(6) 0.1077(6) 0.082(3) Uani 1 1 d . . . . .
F4 F 0.3651(7) 0.6031(5) 0.0342(5) 0.067(3) Uani 1 1 d . . . . .
F5 F 0.2253(12) 1.0206(9) 0.2506(9) 0.140(5) Uani 1 1 d . . . . .
F6 F 0.1594(11) 0.9049(9) 0.2415(8) 0.127(4) Uani 1 1 d . . . . .
N1 N 0.1956(11) 0.9181(7) 0.1475(8) 0.063(3) Uani 1 1 d . . . . .
N2 N 0.3224(17) 0.9248(15) 0.2584(12) 0.128(6) Uani 1 1 d . . . . .
N3 N 0.4201(11) 0.4622(8) 0.3956(7) 0.062(3) Uani 1 1 d . . . . .
N4 N 0.6059(10) 0.5581(8) 0.4856(7) 0.060(3) Uani 1 1 d . . . . .
C1 C 0.7486(11) 0.6145(8) -0.0798(8) 0.051(4) Uani 1 1 d . . . . .
C2 C 0.7260(14) 0.5390(8) -0.0842(11) 0.073(5) Uani 1 1 d . . . . .
H2 H 0.6775 0.5229 -0.0708 0.088 Uiso 1 1 calc R . . . .
C3 C 0.7715(13) 0.4880(11) -0.1072(11) 0.081(6) Uani 1 1 d . . . . .
H3 H 0.7577 0.4362 -0.1078 0.097 Uiso 1 1 calc R . . . .
C4 C 0.8366(13) 0.5086(10) -0.1296(10) 0.071(5) Uani 1 1 d . . . . .
H4 H 0.8643 0.4694 -0.1492 0.085 Uiso 1 1 calc R . . . .
C5 C 0.8650(13) 0.5824(8) -0.1256(10) 0.068(5) Uani 1 1 d . . . . .
H5 H 0.9153 0.5978 -0.1376 0.081 Uiso 1 1 calc R . . . .
C6 C 0.8158(12) 0.6330(10) -0.1031(9) 0.065(5) Uani 1 1 d . . . . .
H6 H 0.8289 0.6843 -0.1036 0.078 Uiso 1 1 calc R . . . .
C7 C 0.7121(11) 0.7690(9) -0.0678(9) 0.051(3) Uani 1 1 d . . . . .
C8 C 0.7576(14) 0.8411(10) -0.0098(11) 0.070(5) Uani 1 1 d . . . . .
H8 H 0.7722 0.8410 0.0363 0.084 Uiso 1 1 calc R . . . .
C9 C 0.7811(16) 0.9097(11) -0.0173(11) 0.085(6) Uani 1 1 d . . . . .
H9 H 0.8124 0.9568 0.0226 0.102 Uiso 1 1 calc R . . . .
C10 C 0.7571(17) 0.9091(11) -0.0874(11) 0.092(7) Uani 1 1 d . . . . .
H10 H 0.7684 0.9564 -0.0956 0.110 Uiso 1 1 calc R . . . .
C11 C 0.7173(16) 0.8383(10) -0.1423(11) 0.088(6) Uani 1 1 d . . . . .
H11 H 0.7039 0.8373 -0.1887 0.105 Uiso 1 1 calc R . . . .
C12 C 0.6965(12) 0.7706(9) -0.1339(9) 0.054(4) Uani 1 1 d . . . . .
H12 H 0.6708 0.7231 -0.1737 0.065 Uiso 1 1 calc R . . . .
C13 C 0.5588(12) 0.6364(10) -0.1248(9) 0.059(4) Uani 1 1 d . . . . .
H13A H 0.5571 0.6511 -0.1653 0.071 Uiso 1 1 calc R . . . .
H13B H 0.5463 0.5786 -0.1403 0.071 Uiso 1 1 calc R . . . .
C14 C 0.4801(12) 0.6642(11) -0.1018(9) 0.063(4) Uani 1 1 d . . . . .
H14A H 0.4170 0.6337 -0.1380 0.076 Uiso 1 1 calc R . . . .
H14B H 0.4847 0.7205 -0.0936 0.076 Uiso 1 1 calc R . . . .
C15 C 0.4483(11) 0.7097(9) 0.0251(9) 0.051(4) Uani 1 1 d . . . . .
C16 C 0.4749(13) 0.7895(10) 0.0456(10) 0.065(5) Uani 1 1 d . . . . .
C17 C 0.4345(15) 0.8388(11) 0.0804(12) 0.079(6) Uani 1 1 d . . . . .
C18 C 0.3702(12) 0.8092(10) 0.1047(10) 0.062(4) Uani 1 1 d . . . . .
C19 C 0.3484(12) 0.7284(10) 0.0875(10) 0.058(4) Uani 1 1 d . . . . .
C20 C 0.3916(13) 0.6793(10) 0.0492(11) 0.066(5) Uani 1 1 d . . . . .
C21 C 0.3242(15) 0.8619(11) 0.1461(11) 0.072(4) Uani 1 1 d . . . . .
C22 C 0.2462(13) 0.8769(8) 0.1119(10) 0.056(3) Uani 1 1 d . . . . .
C23 C 0.1952(14) 0.8636(9) 0.0386(11) 0.066(4) Uani 1 1 d . . . . .
C24 C 0.1138(15) 0.8902(11) 0.0315(12) 0.078(4) Uani 1 1 d . . . . .
C25 C 0.1160(14) 0.9264(10) 0.1000(12) 0.070(4) Uani 1 1 d . . . . .
C26 C 0.374(2) 0.9443(16) 0.3250(15) 0.112(6) Uani 1 1 d . . . . .
C27 C 0.451(2) 0.914(2) 0.3345(16) 0.138(8) Uani 1 1 d . . . . .
C28 C 0.446(2) 0.8740(18) 0.2653(15) 0.123(8) Uani 1 1 d . . . . .
C29 C 0.3692(18) 0.8859(14) 0.2221(13) 0.097(6) Uani 1 1 d . . . . .
C30 C 0.2152(14) 0.8202(10) -0.0235(10) 0.069(5) Uani 1 1 d . . . . .
H30A H 0.2808 0.8407 -0.0145 0.104 Uiso 1 1 calc GR . . . .
H30B H 0.1735 0.8273 -0.0656 0.104 Uiso 1 1 calc GR . . . .
H30C H 0.2045 0.7642 -0.0308 0.104 Uiso 1 1 calc GR . . . .
C31 C 0.0388(15) 0.8906(11) -0.0369(12) 0.083(5) Uani 1 1 d . . . . .
H31A H 0.0078 0.9338 -0.0255 0.100 Uiso 1 1 calc R . . . .
H31B H 0.0690 0.8994 -0.0681 0.100 Uiso 1 1 calc R . . . .
C32 C -0.0308(16) 0.8159(12) -0.0727(13) 0.091(6) Uani 1 1 d . . . . .
H32A H -0.0399 0.7949 -0.1222 0.136 Uiso 1 1 calc GR . . . .
H32B H -0.0905 0.8236 -0.0698 0.136 Uiso 1 1 calc GR . . . .
H32C H -0.0088 0.7789 -0.0501 0.136 Uiso 1 1 calc GR . . . .
C33 C 0.0482(14) 0.9682(11) 0.1192(11) 0.073(5) Uani 1 1 d . . . . .
H33A H 0.0746 0.9968 0.1702 0.109 Uiso 1 1 calc GR . . . .
H33B H -0.0105 0.9301 0.1054 0.109 Uiso 1 1 calc GR . . . .
H33C H 0.0354 1.0052 0.0949 0.109 Uiso 1 1 calc GR . . . .
C34 C 0.354(3) 0.995(2) 0.3805(18) 0.165(12) Uani 1 1 d . . . . .
H34A H 0.3101 1.0246 0.3612 0.247 Uiso 1 1 calc GR . . . .
H34B H 0.4122 1.0316 0.4173 0.247 Uiso 1 1 calc GR . . . .
H34C H 0.3253 0.9633 0.4005 0.247 Uiso 1 1 calc GR . . . .
C35 C 0.514(2) 0.923(2) 0.3970(17) 0.146(8) Uani 1 1 d . . . . .
H35A H 0.5414 0.8767 0.3948 0.176 Uiso 1 1 calc R . . . .
H35B H 0.4854 0.9303 0.4319 0.176 Uiso 1 1 calc R . . . .
C36 C 0.595(3) 1.002(2) 0.4179(16) 0.187(16) Uani 1 1 d . . . . .
H36A H 0.6363 0.9886 0.3933 0.280 Uiso 1 1 calc R . . . .
H36B H 0.6322 1.0233 0.4689 0.280 Uiso 1 1 calc R . . . .
H36C H 0.5645 1.0417 0.4040 0.280 Uiso 1 1 calc R . . . .
C37 C 0.517(2) 0.836(2) 0.2453(14) 0.137(11) Uani 1 1 d . . . . .
H37A H 0.4842 0.7867 0.2053 0.206 Uiso 1 1 calc GR . . . .
H37B H 0.5589 0.8259 0.2853 0.206 Uiso 1 1 calc GR . . . .
H37C H 0.5529 0.8711 0.2322 0.206 Uiso 1 1 calc GR . . . .
C38 C 0.9071(12) 0.6923(10) 0.0940(9) 0.058(4) Uani 1 1 d . . . . .
C39 C 0.9102(12) 0.6168(10) 0.0798(9) 0.057(4) Uani 1 1 d . . . . .
H39 H 0.8679 0.5827 0.0872 0.068 Uiso 1 1 calc R . . . .
C40 C 0.9742(13) 0.5880(11) 0.0544(11) 0.074(5) Uani 1 1 d . . . . .
H40 H 0.9713 0.5334 0.0403 0.088 Uiso 1 1 calc R . . . .
C41 C 1.0430(14) 0.6382(10) 0.0493(11) 0.073(5) Uani 1 1 d . . . . .
H41 H 1.0930 0.6215 0.0383 0.088 Uiso 1 1 calc R . . . .
C42 C 1.0327(13) 0.7148(10) 0.0614(9) 0.061(4) Uani 1 1 d . . . . .
H42 H 1.0737 0.7499 0.0536 0.073 Uiso 1 1 calc R . . . .
C43 C 0.9693(12) 0.7411(10) 0.0829(9) 0.057(4) Uani 1 1 d . . . . .
H43 H 0.9662 0.7941 0.0910 0.069 Uiso 1 1 calc R . . . .
C44 C 0.8526(14) 0.8263(10) 0.1707(10) 0.067(4) Uani 1 1 d . . . . .
C45 C 0.7973(16) 0.8753(11) 0.1696(11) 0.076(4) Uani 1 1 d . . . . .
H45 H 0.7334 0.8533 0.1379 0.091 Uiso 1 1 calc R . . . .
C46 C 0.8220(18) 0.9599(12) 0.2113(12) 0.091(5) Uani 1 1 d . . . . .
H46 H 0.7786 0.9921 0.2059 0.110 Uiso 1 1 calc R . . . .
C47 C 0.924(2) 0.9903(15) 0.2641(14) 0.108(6) Uani 1 1 d . . . . .
H47 H 0.9484 1.0432 0.2958 0.130 Uiso 1 1 calc R . . . .
C48 C 0.9790(19) 0.9394(13) 0.2637(14) 0.102(6) Uani 1 1 d . . . . .
H48 H 1.0430 0.9589 0.2959 0.123 Uiso 1 1 calc R . . . .
C49 C 0.9507(15) 0.8596(12) 0.2201(11) 0.083(5) Uani 1 1 d . . . . .
H49 H 0.9948 0.8278 0.2229 0.100 Uiso 1 1 calc R . . . .
C50 C 0.8241(13) 0.6856(11) 0.1897(9) 0.063(4) Uani 1 1 d . . . . .
H50A H 0.8126 0.6278 0.1707 0.076 Uiso 1 1 calc R . . . .
H50B H 0.8878 0.7072 0.2281 0.076 Uiso 1 1 calc R . . . .
C51 C 0.7477(12) 0.7105(12) 0.2190(9) 0.069(4) Uani 1 1 d . . . . .
H51A H 0.7661 0.7677 0.2458 0.083 Uiso 1 1 calc R . . . .
H51B H 0.7438 0.6833 0.2512 0.083 Uiso 1 1 calc R . . . .
C52 C 0.5928(12) 0.5759(9) 0.1237(9) 0.048(4) Uani 1 1 d . . . . .
H52A H 0.5330 0.5540 0.0813 0.058 Uiso 1 1 calc R . . . .
H52B H 0.6402 0.5484 0.1138 0.058 Uiso 1 1 calc R . . . .
C53 C 0.5787(12) 0.5643(9) 0.1862(9) 0.053(4) Uani 1 1 d . . . . .
C54 C 0.6365(13) 0.5285(11) 0.2280(10) 0.067(5) Uani 1 1 d . . . . .
H54 H 0.6890 0.5138 0.2196 0.080 Uiso 1 1 calc R . . . .
C55 C 0.6169(14) 0.5160(11) 0.2783(10) 0.073(5) Uani 1 1 d . . . . .
H55 H 0.6541 0.4886 0.3034 0.087 Uiso 1 1 calc R . . . .
C56 C 0.5471(13) 0.5391(10) 0.2973(9) 0.065(4) Uani 1 1 d . . . . .
C57 C 0.4869(13) 0.5762(10) 0.2581(9) 0.063(4) Uani 1 1 d . . . . .
H57 H 0.4350 0.5908 0.2675 0.076 Uiso 1 1 calc R . . . .
C58 C 0.5082(12) 0.5895(9) 0.2057(9) 0.055(4) Uani 1 1 d . . . . .
H58 H 0.4723 0.6179 0.1811 0.066 Uiso 1 1 calc R . . . .
C59 C 0.5285(13) 0.5267(10) 0.3588(9) 0.060(4) Uani 1 1 d . . . . .
C60 C 0.4419(13) 0.4790(9) 0.3440(9) 0.055(4) Uani 1 1 d . . . . .
C61 C 0.3698(13) 0.4386(11) 0.2779(9) 0.068(5) Uani 1 1 d . . . . .
H61 H 0.3694 0.4386 0.2341 0.082 Uiso 1 1 calc R . . . .
C62 C 0.3022(14) 0.4004(11) 0.2877(9) 0.068(5) Uani 1 1 d . . . . .
H62 H 0.2423 0.3699 0.2527 0.081 Uiso 1 1 calc R . . . .
C63 C 0.3362(15) 0.4135(11) 0.3611(10) 0.074(5) Uani 1 1 d . . . . .
C64 C 0.6915(13) 0.6065(9) 0.5397(9) 0.059(4) Uani 1 1 d . . . . .
C65 C 0.7431(13) 0.6430(10) 0.5073(9) 0.061(4) Uani 1 1 d . . . . .
H65 H 0.8034 0.6784 0.5308 0.074 Uiso 1 1 calc R . . . .
C66 C 0.6883(13) 0.6164(11) 0.4374(10) 0.072(5) Uani 1 1 d . . . . .
H66 H 0.7038 0.6300 0.4031 0.086 Uiso 1 1 calc R . . . .
C67 C 0.6040(12) 0.5651(9) 0.4242(9) 0.056(4) Uani 1 1 d . . . . .
C68 C 0.2769(14) 0.3796(11) 0.3907(9) 0.070(5) Uani 1 1 d . . . . .
C69 C 0.1851(15) 0.3251(12) 0.3417(10) 0.074(4) Uani 1 1 d . . . . .
C70 C 0.1028(16) 0.3537(12) 0.3233(11) 0.080(4) Uani 1 1 d . . . . .
C71 C 0.0204(18) 0.3008(14) 0.2846(14) 0.110(6) Uani 1 1 d . . . . .
H71 H -0.0358 0.3187 0.2745 0.132 Uiso 1 1 calc R . . . .
C72 C 0.014(2) 0.2191(15) 0.2580(14) 0.111(7) Uani 1 1 d . . . . .
C73 C 0.0860(19) 0.1920(14) 0.2726(11) 0.096(5) Uani 1 1 d . . . . .
H73 H 0.0822 0.1374 0.2549 0.115 Uiso 1 1 calc R . . . .
C74 C 0.1773(16) 0.2500(12) 0.3189(10) 0.079(4) Uani 1 1 d . . . . .
C75 C 0.1156(15) 0.4399(12) 0.3558(13) 0.093(6) Uani 1 1 d . . . . .
H75A H 0.0723 0.4501 0.3791 0.139 Uiso 1 1 calc GR . . . .
H75B H 0.1025 0.4626 0.3191 0.139 Uiso 1 1 calc GR . . . .
H75C H 0.1805 0.4636 0.3905 0.139 Uiso 1 1 calc GR . . . .
C76 C -0.0775(19) 0.1569(16) 0.2116(15) 0.129(8) Uani 1 1 d . . . . .
H76A H -0.1038 0.1619 0.1655 0.194 Uiso 1 1 calc GR . . . .
H76B H -0.1224 0.1638 0.2338 0.194 Uiso 1 1 calc GR . . . .
H76C H -0.0651 0.1048 0.2055 0.194 Uiso 1 1 calc GR . . . .
C77 C 0.2610(18) 0.2109(12) 0.3340(13) 0.098(6) Uani 1 1 d . . . . .
H77A H 0.3088 0.2345 0.3215 0.148 Uiso 1 1 calc GR . . . .
H77B H 0.2390 0.1546 0.3060 0.148 Uiso 1 1 calc GR . . . .
H77C H 0.2884 0.2189 0.3842 0.148 Uiso 1 1 calc GR . . . .
B1 B 0.220(2) 0.9461(18) 0.2190(16) 0.099(5) Uani 1 1 d . . . . .
S3 S 0.2059(10) 0.5771(7) -0.1163(9) 0.153(4) Uani 0.476(9) 1 d . . . A 1
O1 O 0.2580(13) 0.6539(7) -0.1027(11) 0.153(4) Uani 0.476(9) 1 d G . . A 1
O4 O 0.2615(14) 0.5266(11) -0.0912(11) 0.153(4) Uani 0.476(9) 1 d G . . A 1
O5 O 0.1194(12) 0.5746(12) -0.1065(11) 0.153(4) Uani 0.476(9) 1 d G . . A 1
C1A C 0.1637(10) 0.5297(8) -0.2126(9) 0.153(4) Uani 0.476(9) 1 d G . . A 1
F7 F 0.1128(13) 0.4563(8) -0.2363(11) 0.153(4) Uani 0.476(9) 1 d G . . A 1
F8 F 0.1096(14) 0.5684(12) -0.2464(10) 0.153(4) Uani 0.476(9) 1 d G . . A 1
F9 F 0.2347(13) 0.5262(11) -0.2330(11) 0.153(4) Uani 0.476(9) 1 d G . . A 1
C6A C 0.1970(9) 0.5765(7) -0.1541(10) 0.153(4) Uani 0.524(9) 1 d . . . A 2
S3A S 0.1040(8) 0.5963(6) -0.1224(10) 0.153(4) Uani 0.524(9) 1 d G . . A 2
O1A O 0.1504(14) 0.6096(11) -0.0487(10) 0.153(4) Uani 0.524(9) 1 d G . . A 2
O4A O 0.0312(9) 0.5248(9) -0.1640(13) 0.153(4) Uani 0.524(9) 1 d G . . A 2
O5A O 0.0835(12) 0.6643(9) -0.1386(13) 0.153(4) Uani 0.524(9) 1 d G . . A 2
F7A F 0.1675(14) 0.5623(12) -0.2229(10) 0.153(4) Uani 0.524(9) 1 d G . . A 2
F8A F 0.2724(9) 0.6370(9) -0.1214(13) 0.153(4) Uani 0.524(9) 1 d G . . A 2
F9A F 0.2263(12) 0.5142(9) -0.1437(13) 0.153(4) Uani 0.524(9) 1 d G . . A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0659(9) 0.0500(8) 0.0610(9) 0.0277(7) 0.0451(7) 0.0157(6)
Zn1 0.100(3) 0.084(2) 0.060(2) 0.0295(19) 0.050(2) -0.008(2)
S1 0.064(3) 0.056(2) 0.064(3) 0.030(2) 0.045(2) 0.021(2)
S2 0.070(3) 0.053(2) 0.063(3) 0.029(2) 0.044(2) 0.014(2)
P1 0.055(3) 0.043(2) 0.062(3) 0.025(2) 0.038(2) 0.0130(19)
P2 0.065(3) 0.053(2) 0.059(3) 0.025(2) 0.041(2) 0.014(2)
F1 0.101(7) 0.069(6) 0.116(8) 0.040(6) 0.083(7) 0.017(5)
F2 0.142(10) 0.064(5) 0.142(10) 0.029(6) 0.107(9) 0.021(6)
F3 0.093(7) 0.077(6) 0.121(9) 0.045(6) 0.083(7) 0.033(5)
F4 0.096(7) 0.052(4) 0.096(7) 0.041(5) 0.075(6) 0.022(4)
F5 0.171(12) 0.110(8) 0.118(10) 0.000(6) 0.068(9) 0.044(7)
F6 0.131(9) 0.166(10) 0.123(10) 0.061(8) 0.085(8) 0.047(8)
N1 0.075(7) 0.045(7) 0.091(6) 0.023(5) 0.061(5) 0.018(5)
N2 0.133(9) 0.166(14) 0.101(7) 0.034(7) 0.072(6) 0.062(9)
N3 0.085(6) 0.065(7) 0.058(5) 0.030(5) 0.049(5) 0.010(5)
N4 0.084(7) 0.054(7) 0.057(6) 0.027(5) 0.044(5) 0.005(5)
C1 0.066(8) 0.058(6) 0.043(8) 0.025(6) 0.032(7) 0.016(6)
C2 0.081(11) 0.059(7) 0.097(14) 0.036(7) 0.050(11) 0.017(6)
C3 0.086(12) 0.072(8) 0.106(15) 0.043(8) 0.053(12) 0.025(7)
C4 0.078(11) 0.072(8) 0.080(12) 0.036(8) 0.041(10) 0.030(7)
C5 0.078(10) 0.071(8) 0.072(12) 0.031(8) 0.043(10) 0.026(7)
C6 0.081(10) 0.069(8) 0.076(12) 0.043(8) 0.051(10) 0.026(7)
C7 0.059(8) 0.049(6) 0.066(7) 0.025(5) 0.044(6) 0.014(5)
C8 0.085(12) 0.051(6) 0.076(8) 0.019(5) 0.040(8) 0.012(6)
C9 0.116(15) 0.051(7) 0.078(9) 0.018(6) 0.037(9) 0.002(8)
C10 0.133(17) 0.051(7) 0.073(8) 0.025(6) 0.031(9) -0.019(8)
C11 0.132(17) 0.050(7) 0.075(9) 0.026(6) 0.044(9) -0.016(8)
C12 0.064(10) 0.044(7) 0.063(7) 0.022(5) 0.037(7) 0.001(6)
C13 0.070(7) 0.054(8) 0.064(7) 0.024(6) 0.037(5) 0.013(6)
C14 0.061(8) 0.064(10) 0.060(7) 0.017(7) 0.026(6) 0.011(7)
C15 0.051(8) 0.055(5) 0.066(8) 0.033(5) 0.034(7) 0.020(5)
C16 0.083(10) 0.057(6) 0.086(11) 0.035(5) 0.063(10) 0.020(5)
C17 0.092(12) 0.059(6) 0.116(14) 0.032(6) 0.076(12) 0.022(6)
C18 0.065(8) 0.067(6) 0.075(9) 0.031(6) 0.045(8) 0.024(5)
C19 0.057(9) 0.064(6) 0.075(10) 0.032(6) 0.043(9) 0.022(5)
C20 0.070(10) 0.063(6) 0.094(11) 0.039(6) 0.057(10) 0.023(5)
C21 0.079(7) 0.073(9) 0.091(7) 0.034(6) 0.058(6) 0.030(7)
C22 0.065(7) 0.036(7) 0.090(6) 0.024(6) 0.057(5) 0.012(6)
C23 0.082(8) 0.042(8) 0.093(7) 0.026(6) 0.056(6) 0.019(6)
C24 0.088(8) 0.066(10) 0.103(7) 0.032(6) 0.060(6) 0.034(7)
C25 0.079(8) 0.048(9) 0.106(7) 0.026(6) 0.062(6) 0.022(7)
C26 0.132(11) 0.120(15) 0.102(8) 0.040(8) 0.068(7) 0.028(10)
C27 0.150(12) 0.179(19) 0.094(8) 0.038(9) 0.063(8) 0.064(12)
C28 0.128(11) 0.16(2) 0.095(8) 0.044(9) 0.055(8) 0.063(13)
C29 0.105(9) 0.117(14) 0.090(7) 0.038(6) 0.060(6) 0.039(9)
C30 0.094(13) 0.062(10) 0.084(9) 0.040(8) 0.053(9) 0.047(10)
C31 0.094(10) 0.063(9) 0.110(9) 0.033(8) 0.057(7) 0.033(7)
C32 0.104(12) 0.071(10) 0.109(12) 0.038(9) 0.053(10) 0.022(8)
C33 0.095(11) 0.064(10) 0.090(12) 0.035(9) 0.060(10) 0.041(9)
C34 0.19(2) 0.20(3) 0.126(14) 0.038(14) 0.094(16) 0.08(2)
C35 0.159(14) 0.19(2) 0.104(10) 0.060(11) 0.059(9) 0.044(12)
C36 0.21(2) 0.24(3) 0.083(15) 0.081(16) 0.038(16) -0.01(2)
C37 0.128(16) 0.21(3) 0.076(15) 0.043(16) 0.042(13) 0.083(18)
C38 0.066(8) 0.056(6) 0.073(10) 0.031(6) 0.044(8) 0.018(6)
C39 0.064(9) 0.057(7) 0.063(11) 0.030(7) 0.035(9) 0.014(6)
C40 0.076(10) 0.062(8) 0.098(14) 0.029(8) 0.052(11) 0.018(7)
C41 0.077(10) 0.058(7) 0.100(15) 0.022(8) 0.058(11) 0.016(7)
C42 0.069(9) 0.061(7) 0.070(12) 0.024(8) 0.047(9) 0.015(7)
C43 0.067(9) 0.056(7) 0.070(11) 0.029(7) 0.046(9) 0.017(6)
C44 0.089(8) 0.061(6) 0.071(8) 0.023(5) 0.058(7) 0.011(5)
C45 0.109(10) 0.067(7) 0.072(10) 0.022(7) 0.063(8) 0.020(7)
C46 0.132(12) 0.067(8) 0.090(12) 0.021(7) 0.071(10) 0.017(7)
C47 0.130(12) 0.088(10) 0.110(13) 0.019(9) 0.071(10) 0.007(8)
C48 0.112(12) 0.080(9) 0.103(12) 0.012(8) 0.056(9) 0.000(7)
C49 0.089(9) 0.084(9) 0.082(10) 0.018(7) 0.054(7) 0.006(6)
C50 0.067(8) 0.073(9) 0.060(8) 0.027(7) 0.039(7) 0.003(7)
C51 0.072(7) 0.087(11) 0.060(7) 0.035(7) 0.039(6) 0.004(7)
C52 0.056(9) 0.050(7) 0.064(7) 0.034(6) 0.040(7) 0.018(6)
C53 0.065(8) 0.050(8) 0.055(7) 0.026(6) 0.034(7) 0.003(6)
C54 0.074(9) 0.087(12) 0.074(9) 0.051(9) 0.049(8) 0.025(8)
C55 0.083(10) 0.091(12) 0.068(9) 0.044(9) 0.047(8) 0.017(9)
C56 0.084(9) 0.075(10) 0.060(7) 0.041(7) 0.044(7) 0.011(7)
C57 0.072(9) 0.073(10) 0.065(8) 0.041(8) 0.042(7) 0.004(8)
C58 0.073(9) 0.054(9) 0.059(8) 0.033(7) 0.042(7) 0.006(7)
C59 0.083(7) 0.063(8) 0.057(6) 0.037(5) 0.043(5) 0.010(6)
C60 0.080(7) 0.060(8) 0.048(6) 0.030(5) 0.042(5) 0.013(6)
C61 0.078(8) 0.090(11) 0.052(6) 0.031(6) 0.043(5) 0.010(7)
C62 0.087(8) 0.080(10) 0.055(6) 0.030(6) 0.048(6) 0.010(7)
C63 0.098(7) 0.081(10) 0.054(6) 0.025(6) 0.051(6) -0.003(7)
C64 0.084(8) 0.050(8) 0.059(7) 0.023(6) 0.046(6) 0.010(6)
C65 0.080(8) 0.058(9) 0.061(7) 0.026(7) 0.043(6) 0.011(7)
C66 0.083(8) 0.082(11) 0.062(7) 0.032(7) 0.043(6) 0.001(7)
C67 0.072(7) 0.059(8) 0.058(5) 0.028(5) 0.046(5) 0.009(6)
C68 0.094(8) 0.071(9) 0.056(8) 0.022(6) 0.050(7) -0.006(7)
C69 0.096(7) 0.075(7) 0.058(9) 0.026(6) 0.048(7) -0.010(6)
C70 0.096(8) 0.075(7) 0.071(10) 0.024(7) 0.046(7) -0.010(6)
C71 0.099(9) 0.099(9) 0.109(13) 0.026(8) 0.040(8) -0.020(7)
C72 0.107(10) 0.093(9) 0.107(14) 0.025(8) 0.039(9) -0.023(7)
C73 0.122(9) 0.090(9) 0.068(10) 0.023(8) 0.049(8) -0.020(7)
C74 0.111(9) 0.074(7) 0.060(9) 0.025(6) 0.054(7) -0.013(6)
C75 0.076(12) 0.081(8) 0.100(15) 0.024(8) 0.028(11) -0.014(7)
C76 0.122(12) 0.116(14) 0.113(15) 0.028(12) 0.037(11) -0.034(10)
C77 0.131(11) 0.070(11) 0.092(14) 0.021(10) 0.057(10) -0.003(9)
B1 0.118(9) 0.103(9) 0.091(7) 0.020(6) 0.070(6) 0.038(7)
S3 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O1 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O4 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O5 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
C1A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F7 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F8 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F9 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
C6A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
S3A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O1A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O4A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
O5A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F7A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F8A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
F9A 0.117(6) 0.103(5) 0.274(11) 0.075(6) 0.104(7) 0.058(4)
_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
Rh1 S1 2.331(5) . ?
Rh1 S2 2.333(4) . ?
Rh1 P1 2.244(4) . ?
Rh1 P2 2.242(5) . ?
Zn1 N3 2.022(15) 2_666 ?
Zn1 N3 2.022(15) . ?
Zn1 N4 2.038(12) 2_666 ?
Zn1 N4 2.038(12) . ?
S1 C14 1.828(19) . ?
S1 C15 1.772(16) . ?
S2 C51 1.82(2) . ?
S2 C52 1.892(15) . ?
P1 C1 1.837(16) . ?
P1 C7 1.827(15) . ?
P1 C13 1.869(18) . ?
P2 C38 1.816(16) . ?
P2 C44 1.780(19) . ?
P2 C50 1.801(17) . ?
F1 C16 1.386(17) . ?
F2 C17 1.34(2) . ?
F3 C19 1.332(17) . ?
F4 C20 1.324(19) . ?
F5 B1 1.31(3) . ?
F6 B1 1.44(3) . ?
N1 C22 1.42(2) . ?
N1 C25 1.37(3) . ?
N1 B1 1.38(3) . ?
N2 C26 1.30(3) . ?
N2 C29 1.36(3) . ?
N2 B1 1.69(4) . ?
N3 C60 1.387(19) . ?
N3 C63 1.32(2) . ?
N4 C64 1.41(2) . ?
N4 C67 1.37(2) . ?
C1 C2 1.362(13) . ?
C1 C6 1.369(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.325(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.336(14) . ?
C4 H4 0.9500 . ?
C4 C5 1.352(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.359(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.42(2) . ?
C7 C12 1.38(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.35(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.44(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.37(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.34(2) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.56(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.37(2) . ?
C15 C20 1.33(2) . ?
C16 C17 1.36(2) . ?
C17 C18 1.42(2) . ?
C18 C19 1.39(2) . ?
C18 C21 1.53(2) . ?
C19 C20 1.43(2) . ?
C21 C22 1.30(3) . ?
C21 C29 1.45(3) . ?
C22 C23 1.44(3) . ?
C23 C24 1.39(3) . ?
C23 C30 1.50(2) . ?
C24 C25 1.42(3) . ?
C24 C31 1.55(3) . ?
C25 C33 1.48(2) . ?
C26 C27 1.36(4) . ?
C26 C34 1.44(4) . ?
C27 C28 1.43(4) . ?
C27 C35 1.32(4) . ?
C28 C29 1.33(3) . ?
C28 C37 1.49(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.46(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.66(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.34(2) . ?
C38 C43 1.38(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.38(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.40(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.39(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.32(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.32(3) . ?
C44 C49 1.46(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.47(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.53(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.34(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.41(3) . ?
C49 H49 0.9500 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.59(2) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.52(2) . ?
C53 C54 1.42(3) . ?
C53 C58 1.39(2) . ?
C54 H54 0.9500 . ?
C54 C55 1.31(2) . ?
C55 H55 0.9500 . ?
C55 C56 1.36(3) . ?
C56 C57 1.42(3) . ?
C56 C59 1.54(2) . ?
C57 H57 0.9500 . ?
C57 C58 1.37(2) . ?
C58 H58 0.9500 . ?
C59 C60 1.40(2) . ?
C59 C67 1.40(2) . ?
C60 C61 1.39(2) . ?
C61 H61 0.9500 . ?
C61 C62 1.32(2) . ?
C62 H62 0.9500 . ?
C62 C63 1.43(3) . ?
C63 C68 1.48(2) . ?
C64 C65 1.47(2) . ?
C64 C68 1.35(3) 2_666 ?
C65 H65 0.9500 . ?
C65 C66 1.36(3) . ?
C66 H66 0.9500 . ?
C66 C67 1.42(2) . ?
C68 C64 1.35(3) 2_666 ?
C68 C69 1.48(3) . ?
C69 C70 1.42(3) . ?
C69 C74 1.30(3) . ?
C70 C71 1.34(3) . ?
C70 C75 1.49(3) . ?
C71 H71 0.9500 . ?
C71 C72 1.42(4) . ?
C72 C73 1.27(3) . ?
C72 C76 1.52(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.49(3) . ?
C74 C77 1.55(3) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
S3 O1 1.4427 . ?
S3 O4 1.4415 . ?
S3 O5 1.4379 . ?
S3 C1A 1.8446 . ?
C1A F7 1.3360 . ?
C1A F8 1.3351 . ?
C1A F9 1.3312 . ?
C6A S3A 1.8402 . ?
C6A F7A 1.3333 . ?
C6A F8A 1.3361 . ?
C6A F9A 1.3354 . ?
S3A O1A 1.4401 . ?
S3A O4A 1.4434 . ?
S3A O5A 1.4421 . ?
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
S1 Rh1 S2 89.48(15) . . ?
P1 Rh1 S1 85.65(15) . . ?
P1 Rh1 S2 173.90(16) . . ?
P2 Rh1 S1 174.75(14) . . ?
P2 Rh1 S2 85.74(16) . . ?
P2 Rh1 P1 98.98(15) . . ?
N3 Zn1 N3 180.0(5) 2_666 . ?
N3 Zn1 N4 90.1(5) . 2_666 ?
N3 Zn1 N4 89.9(5) . . ?
N3 Zn1 N4 89.9(5) 2_666 2_666 ?
N3 Zn1 N4 90.1(5) 2_666 . ?
N4 Zn1 N4 180.0 2_666 . ?
C14 S1 Rh1 108.1(6) . . ?
C15 S1 Rh1 106.5(6) . . ?
C15 S1 C14 105.5(8) . . ?
C51 S2 Rh1 107.0(5) . . ?
C51 S2 C52 102.8(8) . . ?
C52 S2 Rh1 102.6(5) . . ?
C1 P1 Rh1 117.0(5) . . ?
C1 P1 C13 103.1(7) . . ?
C7 P1 Rh1 120.7(5) . . ?
C7 P1 C1 105.7(6) . . ?
C7 P1 C13 100.4(8) . . ?
C13 P1 Rh1 107.2(5) . . ?
C38 P2 Rh1 123.5(6) . . ?
C44 P2 Rh1 111.3(7) . . ?
C44 P2 C38 109.1(8) . . ?
C44 P2 C50 100.8(8) . . ?
C50 P2 Rh1 106.2(6) . . ?
C50 P2 C38 103.1(8) . . ?
C25 N1 C22 110.1(16) . . ?
C25 N1 B1 123.2(17) . . ?
B1 N1 C22 127(2) . . ?
C26 N2 C29 107(2) . . ?
C26 N2 B1 130(2) . . ?
C29 N2 B1 123(2) . . ?
C60 N3 Zn1 128.3(12) . . ?
C63 N3 Zn1 127.2(10) . . ?
C63 N3 C60 104.5(14) . . ?
C64 N4 Zn1 125.2(10) . . ?
C67 N4 Zn1 127.3(12) . . ?
C67 N4 C64 107.1(12) . . ?
C2 C1 P1 117.6(10) . . ?
C2 C1 C6 117.1(14) . . ?
C6 C1 P1 125.0(11) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(16) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.8(17) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 118.5 . . ?
C3 C4 C5 123.1(16) . . ?
C5 C4 H4 118.5 . . ?
C4 C5 H5 122.7 . . ?
C4 C5 C6 114.5(15) . . ?
C6 C5 H5 122.7 . . ?
C1 C6 H6 118.0 . . ?
C5 C6 C1 124.1(15) . . ?
C5 C6 H6 118.0 . . ?
C8 C7 P1 119.4(13) . . ?
C12 C7 P1 123.7(12) . . ?
C12 C7 C8 116.9(14) . . ?
C7 C8 H8 118.5 . . ?
C9 C8 C7 123.1(19) . . ?
C9 C8 H8 118.5 . . ?
C8 C9 H9 121.1 . . ?
C8 C9 C10 117.8(18) . . ?
C10 C9 H9 121.1 . . ?
C9 C10 H10 121.0 . . ?
C11 C10 C9 118.1(17) . . ?
C11 C10 H10 121.0 . . ?
C10 C11 H11 118.4 . . ?
C12 C11 C10 123.3(19) . . ?
C12 C11 H11 118.4 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.7(16) . . ?
C11 C12 H12 119.7 . . ?
P1 C13 H13A 109.2 . . ?
P1 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 P1 112.1(11) . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
S1 C14 H14A 110.9 . . ?
S1 C14 H14B 110.9 . . ?
C13 C14 S1 104.4(12) . . ?
C13 C14 H14A 110.9 . . ?
C13 C14 H14B 110.9 . . ?
H14A C14 H14B 108.9 . . ?
C16 C15 S1 122.2(11) . . ?
C20 C15 S1 117.9(13) . . ?
C20 C15 C16 119.0(15) . . ?
C15 C16 F1 121.5(14) . . ?
C17 C16 F1 115.4(14) . . ?
C17 C16 C15 122.7(14) . . ?
F2 C17 C16 122.6(15) . . ?
F2 C17 C18 117.1(15) . . ?
C16 C17 C18 120.0(16) . . ?
C17 C18 C21 122.7(16) . . ?
C19 C18 C17 116.4(15) . . ?
C19 C18 C21 120.9(14) . . ?
F3 C19 C18 119.2(13) . . ?
F3 C19 C20 120.0(14) . . ?
C18 C19 C20 120.8(14) . . ?
F4 C20 C15 123.2(15) . . ?
F4 C20 C19 116.4(13) . . ?
C15 C20 C19 120.2(16) . . ?
C22 C21 C18 119.1(18) . . ?
C22 C21 C29 125.1(18) . . ?
C29 C21 C18 115.6(19) . . ?
N1 C22 C23 105.5(16) . . ?
C21 C22 N1 121.3(18) . . ?
C21 C22 C23 133.1(16) . . ?
C22 C23 C30 128.6(17) . . ?
C24 C23 C22 108.3(16) . . ?
C24 C23 C30 122.7(19) . . ?
C23 C24 C25 108(2) . . ?
C23 C24 C31 127.0(18) . . ?
C25 C24 C31 124.4(17) . . ?
N1 C25 C24 107.7(15) . . ?
N1 C25 C33 124.5(18) . . ?
C24 C25 C33 128(2) . . ?
N2 C26 C27 111(3) . . ?
N2 C26 C34 124(3) . . ?
C27 C26 C34 125(3) . . ?
C26 C27 C28 106(3) . . ?
C35 C27 C26 123(3) . . ?
C35 C27 C28 131(3) . . ?
C27 C28 C37 128(3) . . ?
C29 C28 C27 105(2) . . ?
C29 C28 C37 127(2) . . ?
N2 C29 C21 116(2) . . ?
C28 C29 N2 111(2) . . ?
C28 C29 C21 133(2) . . ?
C23 C30 H30A 109.5 . . ?
C23 C30 H30B 109.5 . . ?
C23 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C31 H31A 109.8 . . ?
C24 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 C24 109.4(18) . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C25 C33 H33A 109.5 . . ?
C25 C33 H33B 109.5 . . ?
C25 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C27 C35 H35A 110.8 . . ?
C27 C35 H35B 110.8 . . ?
C27 C35 C36 105(3) . . ?
H35A C35 H35B 108.9 . . ?
C36 C35 H35A 110.8 . . ?
C36 C35 H35B 110.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C28 C37 H37A 109.5 . . ?
C28 C37 H37B 109.5 . . ?
C28 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 P2 118.1(12) . . ?
C39 C38 C43 118.7(15) . . ?
C43 C38 P2 123.0(13) . . ?
C38 C39 H39 119.5 . . ?
C38 C39 C40 121.0(15) . . ?
C40 C39 H39 119.5 . . ?
C39 C40 H40 119.6 . . ?
C39 C40 C41 120.7(17) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 H41 122.5 . . ?
C42 C41 C40 115.0(16) . . ?
C42 C41 H41 122.5 . . ?
C41 C42 H42 118.3 . . ?
C43 C42 C41 123.4(15) . . ?
C43 C42 H42 118.3 . . ?
C38 C43 H43 119.7 . . ?
C42 C43 C38 120.7(16) . . ?
C42 C43 H43 119.7 . . ?
C45 C44 P2 125.3(17) . . ?
C45 C44 C49 116.1(18) . . ?
C49 C44 P2 118.5(16) . . ?
C44 C45 H45 115.8 . . ?
C44 C45 C46 128(2) . . ?
C46 C45 H45 115.8 . . ?
C45 C46 H46 123.5 . . ?
C45 C46 C47 113(2) . . ?
C47 C46 H46 123.5 . . ?
C46 C47 H47 121.4 . . ?
C48 C47 C46 117(2) . . ?
C48 C47 H47 121.4 . . ?
C47 C48 H48 116.9 . . ?
C47 C48 C49 126(3) . . ?
C49 C48 H48 116.9 . . ?
C44 C49 H49 120.5 . . ?
C48 C49 C44 119(2) . . ?
C48 C49 H49 120.5 . . ?
P2 C50 H50A 110.1 . . ?
P2 C50 H50B 110.1 . . ?
H50A C50 H50B 108.4 . . ?
C51 C50 P2 108.0(13) . . ?
C51 C50 H50A 110.1 . . ?
C51 C50 H50B 110.1 . . ?
S2 C51 H51A 109.8 . . ?
S2 C51 H51B 109.8 . . ?
C50 C51 S2 109.5(12) . . ?
C50 C51 H51A 109.8 . . ?
C50 C51 H51B 109.8 . . ?
H51A C51 H51B 108.2 . . ?
S2 C52 H52A 110.0 . . ?
S2 C52 H52B 110.0 . . ?
H52A C52 H52B 108.4 . . ?
C53 C52 S2 108.3(10) . . ?
C53 C52 H52A 110.0 . . ?
C53 C52 H52B 110.0 . . ?
C54 C53 C52 122.3(14) . . ?
C58 C53 C52 121.2(16) . . ?
C58 C53 C54 116.4(14) . . ?
C53 C54 H54 120.4 . . ?
C55 C54 C53 119.1(17) . . ?
C55 C54 H54 120.4 . . ?
C54 C55 H55 117.5 . . ?
C54 C55 C56 125(2) . . ?
C56 C55 H55 117.5 . . ?
C55 C56 C57 118.7(15) . . ?
C55 C56 C59 123.8(18) . . ?
C57 C56 C59 117.5(16) . . ?
C56 C57 H57 122.1 . . ?
C58 C57 C56 115.8(16) . . ?
C58 C57 H57 122.1 . . ?
C53 C58 H58 117.7 . . ?
C57 C58 C53 124.6(18) . . ?
C57 C58 H58 117.7 . . ?
C60 C59 C56 118.4(16) . . ?
C67 C59 C56 113.6(14) . . ?
C67 C59 C60 128.0(13) . . ?
N3 C60 C59 122.6(16) . . ?
N3 C60 C61 110.6(14) . . ?
C61 C60 C59 126.7(13) . . ?
C60 C61 H61 126.6 . . ?
C62 C61 C60 106.9(15) . . ?
C62 C61 H61 126.6 . . ?
C61 C62 H62 126.6 . . ?
C61 C62 C63 106.9(17) . . ?
C63 C62 H62 126.6 . . ?
N3 C63 C62 111.0(14) . . ?
N3 C63 C68 127.7(16) . . ?
C62 C63 C68 121.1(17) . . ?
N4 C64 C65 107.4(14) . . ?
C68 C64 N4 128.4(14) 2_666 . ?
C68 C64 C65 124.1(17) 2_666 . ?
C64 C65 H65 126.6 . . ?
C66 C65 C64 106.9(16) . . ?
C66 C65 H65 126.6 . . ?
C65 C66 H66 125.7 . . ?
C65 C66 C67 108.6(15) . . ?
C67 C66 H66 125.7 . . ?
N4 C67 C59 123.9(14) . . ?
N4 C67 C66 110.0(16) . . ?
C59 C67 C66 126.1(14) . . ?
C64 C68 C63 121.1(17) 2_666 . ?
C64 C68 C69 120.3(14) 2_666 . ?
C69 C68 C63 118.5(15) . . ?
C70 C69 C68 120.3(19) . . ?
C74 C69 C68 121(2) . . ?
C74 C69 C70 119(2) . . ?
C69 C70 C75 116.3(19) . . ?
C71 C70 C69 118(2) . . ?
C71 C70 C75 126(2) . . ?
C70 C71 H71 118.8 . . ?
C70 C71 C72 122(3) . . ?
C72 C71 H71 118.8 . . ?
C71 C72 C76 125(3) . . ?
C73 C72 C71 121(3) . . ?
C73 C72 C76 114(3) . . ?
C72 C73 H73 121.8 . . ?
C72 C73 C74 116(2) . . ?
C74 C73 H73 121.8 . . ?
C69 C74 C73 123(2) . . ?
C69 C74 C77 124(2) . . ?
C73 C74 C77 112.5(19) . . ?
C70 C75 H75A 109.5 . . ?
C70 C75 H75B 109.5 . . ?
C70 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C72 C76 H76A 109.5 . . ?
C72 C76 H76B 109.5 . . ?
C72 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C74 C77 H77A 109.5 . . ?
C74 C77 H77B 109.5 . . ?
C74 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
F5 B1 F6 104.5(18) . . ?
F5 B1 N1 118(3) . . ?
F5 B1 N2 109(2) . . ?
F6 B1 N2 100(2) . . ?
N1 B1 F6 115(2) . . ?
N1 B1 N2 108.2(18) . . ?
O1 S3 C1A 102.5 . . ?
O4 S3 O1 115.6 . . ?
O4 S3 C1A 102.5 . . ?
O5 S3 O1 115.5 . . ?
O5 S3 O4 115.5 . . ?
O5 S3 C1A 102.1 . . ?
F7 C1A S3 112.0 . . ?
F8 C1A S3 112.0 . . ?
F8 C1A F7 107.0 . . ?
F9 C1A S3 111.6 . . ?
F9 C1A F7 107.0 . . ?
F9 C1A F8 107.0 . . ?
F7A C6A S3A 111.7 . . ?
F7A C6A F8A 107.1 . . ?
F7A C6A F9A 107.0 . . ?
F8A C6A S3A 111.9 . . ?
F9A C6A S3A 111.9 . . ?
F9A C6A F8A 107.0 . . ?
O1A S3A C6A 102.2 . . ?
O1A S3A O4A 115.6 . . ?
O1A S3A O5A 115.5 . . ?
O4A S3A C6A 102.5 . . ?
O5A S3A C6A 102.4 . . ?
O5A S3A O4A 115.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 S1 C14 C13 43.8(12) . . . . ?
Rh1 S1 C15 C16 54.1(16) . . . . ?
Rh1 S1 C15 C20 -115.0(15) . . . . ?
Rh1 S2 C51 C50 -28.4(13) . . . . ?
Rh1 S2 C52 C53 175.5(10) . . . . ?
Rh1 P1 C1 C2 52.7(16) . . . . ?
Rh1 P1 C1 C6 -134.1(14) . . . . ?
Rh1 P1 C7 C8 20.2(15) . . . . ?
Rh1 P1 C7 C12 -160.2(12) . . . . ?
Rh1 P1 C13 C14 36.3(13) . . . . ?
Rh1 P2 C38 C39 -70.3(16) . . . . ?
Rh1 P2 C38 C43 105.2(15) . . . . ?
Rh1 P2 C44 C45 4.9(17) . . . . ?
Rh1 P2 C44 C49 -179.3(11) . . . . ?
Rh1 P2 C50 C51 -49.7(12) . . . . ?
Zn1 N3 C60 C59 1(2) . . . . ?
Zn1 N3 C60 C61 177.2(12) . . . . ?
Zn1 N3 C63 C62 -179.7(13) . . . . ?
Zn1 N3 C63 C68 5(3) . . . . ?
Zn1 N4 C64 C65 -174.3(11) . . . . ?
Zn1 N4 C64 C68 4(3) . . . 2_666 ?
Zn1 N4 C67 C59 -5(2) . . . . ?
Zn1 N4 C67 C66 174.3(12) . . . . ?
S1 C15 C16 F1 8(3) . . . . ?
S1 C15 C16 C17 -179.8(17) . . . . ?
S1 C15 C20 F4 -8(3) . . . . ?
S1 C15 C20 C19 178.4(15) . . . . ?
S2 C52 C53 C54 -112.1(15) . . . . ?
S2 C52 C53 C58 67.1(17) . . . . ?
P1 C1 C2 C3 176.8(17) . . . . ?
P1 C1 C6 C5 -177.8(15) . . . . ?
P1 C7 C8 C9 -177.0(16) . . . . ?
P1 C7 C12 C11 175.5(16) . . . . ?
P1 C13 C14 S1 -51.0(13) . . . . ?
P2 C38 C39 C40 175.7(15) . . . . ?
P2 C38 C43 C42 -178.1(15) . . . . ?
P2 C44 C45 C46 176.9(15) . . . . ?
P2 C44 C49 C48 -174.8(16) . . . . ?
P2 C50 C51 S2 50.3(14) . . . . ?
F1 C16 C17 F2 -6(3) . . . . ?
F1 C16 C17 C18 -179.1(18) . . . . ?
F2 C17 C18 C19 -176.9(19) . . . . ?
F2 C17 C18 C21 5(3) . . . . ?
F3 C19 C20 F4 2(3) . . . . ?
F3 C19 C20 C15 175.7(17) . . . . ?
N1 C22 C23 C24 -4.8(17) . . . . ?
N1 C22 C23 C30 -177.8(15) . . . . ?
N2 C26 C27 C28 3(4) . . . . ?
N2 C26 C27 C35 -178(4) . . . . ?
N3 C60 C61 C62 3(2) . . . . ?
N3 C63 C68 C64 -4(3) . . . 2_666 ?
N3 C63 C68 C69 -179(2) . . . . ?
N4 C64 C65 C66 0(2) . . . . ?
C1 P1 C7 C8 -115.6(13) . . . . ?
C1 P1 C7 C12 64.0(16) . . . . ?
C1 P1 C13 C14 160.3(12) . . . . ?
C1 C2 C3 C4 -3(3) . . . . ?
C2 C1 C6 C5 -5(3) . . . . ?
C2 C3 C4 C5 5(3) . . . . ?
C3 C4 C5 C6 -6(3) . . . . ?
C4 C5 C6 C1 6(3) . . . . ?
C6 C1 C2 C3 3(3) . . . . ?
C7 P1 C1 C2 -169.6(15) . . . . ?
C7 P1 C1 C6 3.6(18) . . . . ?
C7 P1 C13 C14 -90.7(13) . . . . ?
C7 C8 C9 C10 1(3) . . . . ?
C8 C7 C12 C11 -5(3) . . . . ?
C8 C9 C10 C11 -4(3) . . . . ?
C9 C10 C11 C12 3(4) . . . . ?
C10 C11 C12 C7 2(3) . . . . ?
C12 C7 C8 C9 3(3) . . . . ?
C13 P1 C1 C2 -64.6(16) . . . . ?
C13 P1 C1 C6 108.6(16) . . . . ?
C13 P1 C7 C8 137.5(13) . . . . ?
C13 P1 C7 C12 -42.9(15) . . . . ?
C14 S1 C15 C16 -60.7(17) . . . . ?
C14 S1 C15 C20 130.2(15) . . . . ?
C15 S1 C14 C13 157.4(11) . . . . ?
C15 C16 C17 F2 -179(2) . . . . ?
C15 C16 C17 C18 8(3) . . . . ?
C16 C15 C20 F4 -177.4(18) . . . . ?
C16 C15 C20 C19 9(3) . . . . ?
C16 C17 C18 C19 -3(3) . . . . ?
C16 C17 C18 C21 178(2) . . . . ?
C17 C18 C19 F3 -178.6(18) . . . . ?
C17 C18 C19 C20 2(3) . . . . ?
C17 C18 C21 C22 88(2) . . . . ?
C17 C18 C21 C29 -97(2) . . . . ?
C18 C19 C20 F4 -178.8(17) . . . . ?
C18 C19 C20 C15 -5(3) . . . . ?
C18 C21 C22 N1 173.1(13) . . . . ?
C18 C21 C22 C23 -11(3) . . . . ?
C18 C21 C29 N2 -173(2) . . . . ?
C18 C21 C29 C28 3(4) . . . . ?
C19 C18 C21 C22 -90(2) . . . . ?
C19 C18 C21 C29 85(2) . . . . ?
C20 C15 C16 F1 176.6(18) . . . . ?
C20 C15 C16 C17 -11(3) . . . . ?
C21 C18 C19 F3 0(3) . . . . ?
C21 C18 C19 C20 -179.8(19) . . . . ?
C21 C22 C23 C24 178.5(19) . . . . ?
C21 C22 C23 C30 6(3) . . . . ?
C22 N1 C25 C24 -0.1(18) . . . . ?
C22 N1 C25 C33 -178.5(15) . . . . ?
C22 N1 B1 F5 126(2) . . . . ?
C22 N1 B1 F6 -110(2) . . . . ?
C22 N1 B1 N2 1(3) . . . . ?
C22 C21 C29 N2 2(3) . . . . ?
C22 C21 C29 C28 178(3) . . . . ?
C22 C23 C24 C25 4.9(19) . . . . ?
C22 C23 C24 C31 177.8(17) . . . . ?
C23 C24 C25 N1 -3(2) . . . . ?
C23 C24 C25 C33 175.3(17) . . . . ?
C23 C24 C31 C32 88(2) . . . . ?
C25 N1 C22 C21 -179.9(16) . . . . ?
C25 N1 C22 C23 3.0(16) . . . . ?
C25 N1 B1 F5 -54(3) . . . . ?
C25 N1 B1 F6 70(3) . . . . ?
C25 N1 B1 N2 -179.3(17) . . . . ?
C25 C24 C31 C32 -101(2) . . . . ?
C26 N2 C29 C21 -177(2) . . . . ?
C26 N2 C29 C28 6(3) . . . . ?
C26 N2 B1 F5 45(4) . . . . ?
C26 N2 B1 F6 -65(3) . . . . ?
C26 N2 B1 N1 175(3) . . . . ?
C26 C27 C28 C29 1(4) . . . . ?
C26 C27 C28 C37 174(3) . . . . ?
C26 C27 C35 C36 -92(4) . . . . ?
C27 C28 C29 N2 -4(3) . . . . ?
C27 C28 C29 C21 -180(3) . . . . ?
C28 C27 C35 C36 87(5) . . . . ?
C29 N2 C26 C27 -5(3) . . . . ?
C29 N2 C26 C34 172(3) . . . . ?
C29 N2 B1 F5 -131(3) . . . . ?
C29 N2 B1 F6 120(2) . . . . ?
C29 N2 B1 N1 0(4) . . . . ?
C29 C21 C22 N1 -2(3) . . . . ?
C29 C21 C22 C23 174.7(19) . . . . ?
C30 C23 C24 C25 178.3(15) . . . . ?
C30 C23 C24 C31 -9(3) . . . . ?
C31 C24 C25 N1 -176.2(16) . . . . ?
C31 C24 C25 C33 2(3) . . . . ?
C34 C26 C27 C28 -174(3) . . . . ?
C34 C26 C27 C35 4(6) . . . . ?
C35 C27 C28 C29 -178(4) . . . . ?
C35 C27 C28 C37 -4(6) . . . . ?
C37 C28 C29 N2 -178(3) . . . . ?
C37 C28 C29 C21 7(5) . . . . ?
C38 P2 C44 C45 144.5(15) . . . . ?
C38 P2 C44 C49 -39.6(16) . . . . ?
C38 P2 C50 C51 179.2(12) . . . . ?
C38 C39 C40 C41 6(3) . . . . ?
C39 C38 C43 C42 -3(3) . . . . ?
C39 C40 C41 C42 -9(3) . . . . ?
C40 C41 C42 C43 7(3) . . . . ?
C41 C42 C43 C38 -1(3) . . . . ?
C43 C38 C39 C40 0(3) . . . . ?
C44 P2 C38 C39 156.0(15) . . . . ?
C44 P2 C38 C43 -28.5(19) . . . . ?
C44 P2 C50 C51 66.5(13) . . . . ?
C44 C45 C46 C47 -3(3) . . . . ?
C45 C44 C49 C48 1(3) . . . . ?
C45 C46 C47 C48 3(3) . . . . ?
C46 C47 C48 C49 -1(4) . . . . ?
C47 C48 C49 C44 -1(3) . . . . ?
C49 C44 C45 C46 1(3) . . . . ?
C50 P2 C38 C39 49.5(17) . . . . ?
C50 P2 C38 C43 -135.0(16) . . . . ?
C50 P2 C44 C45 -107.5(16) . . . . ?
C50 P2 C44 C49 68.4(14) . . . . ?
C51 S2 C52 C53 64.5(12) . . . . ?
C52 S2 C51 C50 79.2(12) . . . . ?
C52 C53 C54 C55 -175.8(16) . . . . ?
C52 C53 C58 C57 175.1(16) . . . . ?
C53 C54 C55 C56 -4(3) . . . . ?
C54 C53 C58 C57 -6(2) . . . . ?
C54 C55 C56 C57 3(3) . . . . ?
C54 C55 C56 C59 -177.2(19) . . . . ?
C55 C56 C57 C58 -4(2) . . . . ?
C55 C56 C59 C60 -117(2) . . . . ?
C55 C56 C59 C67 62(2) . . . . ?
C56 C57 C58 C53 5(3) . . . . ?
C56 C59 C60 N3 177.7(16) . . . . ?
C56 C59 C60 C61 2(3) . . . . ?
C56 C59 C67 N4 -175.4(16) . . . . ?
C56 C59 C67 C66 5(3) . . . . ?
C57 C56 C59 C60 62(2) . . . . ?
C57 C56 C59 C67 -119.1(19) . . . . ?
C58 C53 C54 C55 5(3) . . . . ?
C59 C56 C57 C58 177.1(15) . . . . ?
C59 C60 C61 C62 179.1(18) . . . . ?
C60 N3 C63 C62 -2(2) . . . . ?
C60 N3 C63 C68 -177(2) . . . . ?
C60 C59 C67 N4 3(3) . . . . ?
C60 C59 C67 C66 -176.2(18) . . . . ?
C60 C61 C62 C63 -4(2) . . . . ?
C61 C62 C63 N3 4(2) . . . . ?
C61 C62 C63 C68 179.1(19) . . . . ?
C62 C63 C68 C64 -178.6(19) . . . 2_666 ?
C62 C63 C68 C69 6(3) . . . . ?
C63 N3 C60 C59 -177.0(17) . . . . ?
C63 N3 C60 C61 -1(2) . . . . ?
C63 C68 C69 C70 -92(2) . . . . ?
C63 C68 C69 C74 93(2) . . . . ?
C64 N4 C67 C59 -178.6(17) . . . . ?
C64 N4 C67 C66 1.1(19) . . . . ?
C64 C65 C66 C67 0(2) . . . . ?
C64 C68 C69 C70 93(2) 2_666 . . . ?
C64 C68 C69 C74 -82(2) 2_666 . . . ?
C65 C66 C67 N4 -1(2) . . . . ?
C65 C66 C67 C59 178.7(18) . . . . ?
C67 N4 C64 C65 -0.8(18) . . . . ?
C67 N4 C64 C68 178(2) . . . 2_666 ?
C67 C59 C60 N3 -1(3) . . . . ?
C67 C59 C60 C61 -176.8(19) . . . . ?
C68 C64 C65 C66 -178.4(19) 2_666 . . . ?
C68 C69 C70 C71 -173.3(17) . . . . ?
C68 C69 C70 C75 0(2) . . . . ?
C68 C69 C74 C73 176.7(15) . . . . ?
C68 C69 C74 C77 -6(3) . . . . ?
C69 C70 C71 C72 -4(3) . . . . ?
C70 C69 C74 C73 1(2) . . . . ?
C70 C69 C74 C77 179.2(17) . . . . ?
C70 C71 C72 C73 3(4) . . . . ?
C70 C71 C72 C76 -178(2) . . . . ?
C71 C72 C73 C74 0(4) . . . . ?
C72 C73 C74 C69 -3(3) . . . . ?
C72 C73 C74 C77 180(2) . . . . ?
C74 C69 C70 C71 2(3) . . . . ?
C74 C69 C70 C75 175.4(17) . . . . ?
C75 C70 C71 C72 -177(2) . . . . ?
C76 C72 C73 C74 -179.0(18) . . . . ?
B1 N1 C22 C21 0(3) . . . . ?
B1 N1 C22 C23 -178(2) . . . . ?
B1 N1 C25 C24 -180(2) . . . . ?
B1 N1 C25 C33 2(3) . . . . ?
B1 N2 C26 C27 179(3) . . . . ?
B1 N2 C26 C34 -4(5) . . . . ?
B1 N2 C29 C21 -1(3) . . . . ?
B1 N2 C29 C28 -178(3) . . . . ?
O1 S3 C1A F7 180.0 . . . . ?
O1 S3 C1A F8 -59.9 . . . . ?
O1 S3 C1A F9 60.1 . . . . ?
O4 S3 C1A F7 59.9 . . . . ?
O4 S3 C1A F8 180.0 . . . . ?
O4 S3 C1A F9 -60.0 . . . . ?
O5 S3 C1A F7 -60.1 . . . . ?
O5 S3 C1A F8 60.0 . . . . ?
O5 S3 C1A F9 -180.0 . . . . ?
F7A C6A S3A O1A 180.0 . . . . ?
F7A C6A S3A O4A 59.9 . . . . ?
F7A C6A S3A O5A -60.1 . . . . ?
F8A C6A S3A O1A -60.0 . . . . ?
F8A C6A S3A O4A 180.0 . . . . ?
F8A C6A S3A O5A 60.0 . . . . ?
F9A C6A S3A O1A 60.1 . . . . ?
F9A C6A S3A O4A -60.0 . . . . ?
F9A C6A S3A O5A -180.0 . . . . ?
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement. As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.
Total solvent accessible volume / cell = 2316.2 Ang^3^ [42.6%]
Total electron count / cell = 258.7
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.343 -0.229 -0.014 2316.2 258.7 ?
_shelx_res_file
;
TITL n3560a in P-1
CELL 1.54178 15.6349 18.4356 21.753 107.5167 110.2883 96.4162
ZERR 1 0.0009 0.0012 0.0015 0.0043 0.0038 0.004
LATT 1
SFAC C H B F N O P Rh S Zn
UNIT 156 142 2 18 8 6 4 2 6 1
SADI C2 C1 C3 C2 C4 C3 C5 C4 C6 C5 C6 C1
RIGU
EADP S3 O1 O4 O5 C1A F7 F8 F9
EADP S3 O1 O4 O5 C1A F7 F8 F9 C6A S3A F7A F8A F9A O1A O4A O5A
L.S. 4
PLAN 20
SIZE 0.023 0.063 0.147
TEMP -173.15
REM Solution 1 R1 0.266 Rweak 0.006, Alpha = 0.1023 in P-1
BOND $h
acta
wpdb -2
MORE -1
CONF
fmap 2
REM Z:/Charlotte/n3560a/n3560a_a-mask.hkl
WGHT 0.200000
FVAR 0.30889 0.47629
RH1 8 0.663066 0.688329 0.048592 11.00000 0.06593 0.05001 =
0.06102 0.02765 0.04508 0.01570
ZN1 10 0.500000 0.500000 0.500000 10.50000 0.10040 0.08357 =
0.05989 0.02947 0.04986 -0.00756
S1 9 0.501977 0.646181 -0.020070 11.00000 0.06370 0.05596 =
0.06424 0.02988 0.04509 0.02124
S2 9 0.634169 0.684617 0.145982 11.00000 0.07019 0.05334 =
0.06296 0.02934 0.04390 0.01440
P1 7 0.678260 0.680426 -0.051920 11.00000 0.05528 0.04271 =
0.06207 0.02490 0.03755 0.01301
P2 7 0.815566 0.723705 0.121207 11.00000 0.06546 0.05316 =
0.05944 0.02517 0.04062 0.01365
F1 4 0.537795 0.824628 0.025010 11.00000 0.10094 0.06862 =
0.11598 0.04038 0.08309 0.01720
F2 4 0.459403 0.916579 0.099255 11.00000 0.14242 0.06368 =
0.14164 0.02925 0.10743 0.02145
F3 4 0.286930 0.696871 0.107689 11.00000 0.09256 0.07690 =
0.12069 0.04518 0.08252 0.03274
F4 4 0.365150 0.603125 0.034226 11.00000 0.09582 0.05221 =
0.09603 0.04136 0.07512 0.02190
F5 4 0.225294 1.020628 0.250611 11.00000 0.17130 0.11050 =
0.11800 -0.00045 0.06832 0.04385
F6 4 0.159392 0.904919 0.241531 11.00000 0.13089 0.16576 =
0.12338 0.06118 0.08470 0.04729
N1 5 0.195607 0.918109 0.147502 11.00000 0.07529 0.04484 =
0.09104 0.02305 0.06079 0.01751
N2 5 0.322447 0.924796 0.258357 11.00000 0.13297 0.16636 =
0.10145 0.03433 0.07200 0.06194
N3 5 0.420111 0.462195 0.395592 11.00000 0.08461 0.06468 =
0.05770 0.02953 0.04925 0.00956
N4 5 0.605904 0.558140 0.485604 11.00000 0.08435 0.05423 =
0.05676 0.02729 0.04392 0.00543
C1 1 0.748578 0.614451 -0.079791 11.00000 0.06609 0.05813 =
0.04298 0.02465 0.03156 0.01551
C2 1 0.725976 0.538992 -0.084204 11.00000 0.08052 0.05871 =
0.09742 0.03569 0.04978 0.01679
AFIX 43
H2 2 0.677523 0.522921 -0.070772 11.00000 -1.20000
AFIX 0
C3 1 0.771522 0.488016 -0.107213 11.00000 0.08553 0.07158 =
0.10648 0.04280 0.05316 0.02489
AFIX 43
H3 2 0.757736 0.436235 -0.107811 11.00000 -1.20000
AFIX 0
C4 1 0.836641 0.508571 -0.129597 11.00000 0.07790 0.07179 =
0.07988 0.03565 0.04124 0.02969
AFIX 43
H4 2 0.864268 0.469406 -0.149242 11.00000 -1.20000
AFIX 0
C5 1 0.865048 0.582447 -0.125605 11.00000 0.07785 0.07073 =
0.07197 0.03131 0.04252 0.02604
AFIX 43
H5 2 0.915343 0.597811 -0.137557 11.00000 -1.20000
AFIX 0
C6 1 0.815823 0.632950 -0.103110 11.00000 0.08074 0.06901 =
0.07636 0.04332 0.05119 0.02630
AFIX 43
H6 2 0.828895 0.684304 -0.103597 11.00000 -1.20000
AFIX 0
C7 1 0.712086 0.769033 -0.067762 11.00000 0.05858 0.04866 =
0.06611 0.02542 0.04375 0.01433
C8 1 0.757588 0.841142 -0.009806 11.00000 0.08484 0.05054 =
0.07646 0.01892 0.03953 0.01209
AFIX 43
H8 2 0.772151 0.841042 0.036347 11.00000 -1.20000
AFIX 0
C9 1 0.781070 0.909721 -0.017254 11.00000 0.11590 0.05062 =
0.07757 0.01795 0.03699 0.00152
AFIX 43
H9 2 0.812429 0.956822 0.022579 11.00000 -1.20000
AFIX 0
C10 1 0.757074 0.909121 -0.087391 11.00000 0.13261 0.05065 =
0.07345 0.02527 0.03082 -0.01874
AFIX 43
H10 2 0.768387 0.956386 -0.095552 11.00000 -1.20000
AFIX 0
C11 1 0.717305 0.838269 -0.142327 11.00000 0.13229 0.05000 =
0.07477 0.02599 0.04369 -0.01641
AFIX 43
H11 2 0.703889 0.837310 -0.188673 11.00000 -1.20000
AFIX 0
C12 1 0.696533 0.770624 -0.133874 11.00000 0.06383 0.04408 =
0.06304 0.02232 0.03720 0.00144
AFIX 43
H12 2 0.670803 0.723097 -0.173692 11.00000 -1.20000
AFIX 0
C13 1 0.558798 0.636390 -0.124760 11.00000 0.07000 0.05442 =
0.06357 0.02355 0.03719 0.01328
AFIX 23
H13A 2 0.557138 0.651081 -0.165273 11.00000 -1.20000
H13B 2 0.546325 0.578552 -0.140292 11.00000 -1.20000
AFIX 0
C14 1 0.480092 0.664163 -0.101756 11.00000 0.06139 0.06444 =
0.05966 0.01687 0.02639 0.01092
AFIX 23
H14A 2 0.417018 0.633710 -0.138015 11.00000 -1.20000
H14B 2 0.484653 0.720529 -0.093605 11.00000 -1.20000
AFIX 0
C15 1 0.448317 0.709742 0.025057 11.00000 0.05087 0.05477 =
0.06585 0.03254 0.03351 0.01964
C16 1 0.474944 0.789543 0.045594 11.00000 0.08349 0.05717 =
0.08632 0.03505 0.06259 0.01978
C17 1 0.434470 0.838841 0.080377 11.00000 0.09204 0.05878 =
0.11597 0.03162 0.07575 0.02159
C18 1 0.370171 0.809227 0.104688 11.00000 0.06549 0.06669 =
0.07506 0.03068 0.04464 0.02365
C19 1 0.348414 0.728370 0.087540 11.00000 0.05650 0.06403 =
0.07496 0.03166 0.04287 0.02187
C20 1 0.391615 0.679339 0.049153 11.00000 0.07017 0.06268 =
0.09418 0.03863 0.05678 0.02348
C21 1 0.324240 0.861872 0.146066 11.00000 0.07919 0.07288 =
0.09126 0.03351 0.05838 0.03026
C22 1 0.246220 0.876944 0.111882 11.00000 0.06487 0.03630 =
0.08988 0.02380 0.05675 0.01212
C23 1 0.195202 0.863585 0.038601 11.00000 0.08183 0.04226 =
0.09349 0.02620 0.05629 0.01890
C24 1 0.113809 0.890159 0.031458 11.00000 0.08777 0.06590 =
0.10287 0.03174 0.06013 0.03406
C25 1 0.116045 0.926441 0.099998 11.00000 0.07903 0.04829 =
0.10593 0.02558 0.06244 0.02247
C26 1 0.374209 0.944333 0.325025 11.00000 0.13158 0.11962 =
0.10184 0.04044 0.06819 0.02798
C27 1 0.450845 0.913566 0.334477 11.00000 0.15006 0.17932 =
0.09403 0.03783 0.06340 0.06408
C28 1 0.446190 0.874037 0.265295 11.00000 0.12763 0.16222 =
0.09496 0.04442 0.05532 0.06271
C29 1 0.369212 0.885867 0.222107 11.00000 0.10467 0.11661 =
0.09042 0.03807 0.06019 0.03926
C30 1 0.215245 0.820166 -0.023481 11.00000 0.09391 0.06244 =
0.08426 0.03987 0.05331 0.04739
AFIX 137
H30A 2 0.280778 0.840657 -0.014455 11.00000 -1.50000
H30B 2 0.173491 0.827310 -0.065612 11.00000 -1.50000
H30C 2 0.204527 0.764234 -0.030834 11.00000 -1.50000
AFIX 0
C31 1 0.038780 0.890643 -0.036903 11.00000 0.09377 0.06328 =
0.11006 0.03261 0.05682 0.03263
AFIX 23
H31A 2 0.007771 0.933788 -0.025496 11.00000 -1.20000
H31B 2 0.069007 0.899389 -0.068073 11.00000 -1.20000
AFIX 0
C32 1 -0.030789 0.815880 -0.072673 11.00000 0.10413 0.07124 =
0.10939 0.03848 0.05290 0.02185
AFIX 137
H32A 2 -0.039871 0.794852 -0.122176 11.00000 -1.50000
H32B 2 -0.090505 0.823571 -0.069802 11.00000 -1.50000
H32C 2 -0.008808 0.778904 -0.050112 11.00000 -1.50000
AFIX 0
C33 1 0.048162 0.968170 0.119230 11.00000 0.09473 0.06449 =
0.08977 0.03503 0.06033 0.04149
AFIX 137
H33A 2 0.074622 0.996844 0.170208 11.00000 -1.50000
H33B 2 -0.010485 0.930143 0.105358 11.00000 -1.50000
H33C 2 0.035395 1.005156 0.094861 11.00000 -1.50000
AFIX 0
C34 1 0.353842 0.995029 0.380482 11.00000 0.19193 0.19592 =
0.12559 0.03802 0.09449 0.07595
AFIX 137
H34A 2 0.310141 1.024555 0.361232 11.00000 -1.50000
H34B 2 0.412232 1.031618 0.417332 11.00000 -1.50000
H34C 2 0.325327 0.963325 0.400524 11.00000 -1.50000
AFIX 0
C35 1 0.513932 0.922815 0.396967 11.00000 0.15880 0.18695 =
0.10438 0.05952 0.05922 0.04356
AFIX 23
H35A 2 0.541370 0.876711 0.394808 11.00000 -1.20000
H35B 2 0.485378 0.930256 0.431857 11.00000 -1.20000
AFIX 0
C36 1 0.594981 1.002213 0.417916 11.00000 0.21401 0.24363 =
0.08331 0.08148 0.03761 -0.00796
AFIX 33
H36A 2 0.636286 0.988629 0.393345 11.00000 -1.50000
H36B 2 0.632176 1.023309 0.468854 11.00000 -1.50000
H36C 2 0.564469 1.041712 0.403952 11.00000 -1.50000
AFIX 0
C37 1 0.516525 0.836206 0.245297 11.00000 0.12770 0.21245 =
0.07595 0.04264 0.04205 0.08270
AFIX 137
H37A 2 0.484157 0.786692 0.205260 11.00000 -1.50000
H37B 2 0.558935 0.825858 0.285268 11.00000 -1.50000
H37C 2 0.552897 0.871105 0.232166 11.00000 -1.50000
AFIX 0
C38 1 0.907098 0.692265 0.094041 11.00000 0.06620 0.05589 =
0.07321 0.03061 0.04415 0.01765
C39 1 0.910214 0.616830 0.079761 11.00000 0.06437 0.05659 =
0.06282 0.02978 0.03455 0.01437
AFIX 43
H39 2 0.867876 0.582706 0.087195 11.00000 -1.20000
AFIX 0
C40 1 0.974168 0.587999 0.054371 11.00000 0.07584 0.06200 =
0.09833 0.02914 0.05233 0.01814
AFIX 43
H40 2 0.971255 0.533431 0.040258 11.00000 -1.20000
AFIX 0
C41 1 1.042985 0.638235 0.049254 11.00000 0.07745 0.05751 =
0.09972 0.02201 0.05774 0.01555
AFIX 43
H41 2 1.093032 0.621490 0.038347 11.00000 -1.20000
AFIX 0
C42 1 1.032731 0.714827 0.061356 11.00000 0.06890 0.06091 =
0.07029 0.02423 0.04706 0.01484
AFIX 43
H42 2 1.073658 0.749851 0.053616 11.00000 -1.20000
AFIX 0
C43 1 0.969307 0.741106 0.082939 11.00000 0.06677 0.05595 =
0.06990 0.02887 0.04555 0.01658
AFIX 43
H43 2 0.966217 0.794144 0.090974 11.00000 -1.20000
AFIX 0
C44 1 0.852610 0.826317 0.170652 11.00000 0.08913 0.06123 =
0.07089 0.02346 0.05820 0.01054
C45 1 0.797321 0.875316 0.169578 11.00000 0.10920 0.06686 =
0.07164 0.02174 0.06290 0.01991
AFIX 43
H45 2 0.733382 0.853330 0.137855 11.00000 -1.20000
AFIX 0
C46 1 0.821975 0.959870 0.211293 11.00000 0.13185 0.06742 =
0.09028 0.02110 0.07112 0.01667
AFIX 43
H46 2 0.778642 0.992098 0.205931 11.00000 -1.20000
AFIX 0
C47 1 0.924468 0.990309 0.264059 11.00000 0.12981 0.08789 =
0.10956 0.01935 0.07065 0.00689
AFIX 43
H47 2 0.948430 1.043233 0.295805 11.00000 -1.20000
AFIX 0
C48 1 0.979018 0.939394 0.263706 11.00000 0.11245 0.07966 =
0.10336 0.01178 0.05630 0.00003
AFIX 43
H48 2 1.042978 0.958924 0.295930 11.00000 -1.20000
AFIX 0
C49 1 0.950726 0.859579 0.220130 11.00000 0.08858 0.08374 =
0.08166 0.01812 0.05382 0.00560
AFIX 43
H49 2 0.994766 0.827845 0.222862 11.00000 -1.20000
AFIX 0
C50 1 0.824133 0.685647 0.189742 11.00000 0.06728 0.07253 =
0.06034 0.02665 0.03906 0.00310
AFIX 23
H50A 2 0.812627 0.627818 0.170736 11.00000 -1.20000
H50B 2 0.887791 0.707238 0.228051 11.00000 -1.20000
AFIX 0
C51 1 0.747744 0.710457 0.219014 11.00000 0.07175 0.08737 =
0.06031 0.03482 0.03911 0.00435
AFIX 23
H51A 2 0.766130 0.767654 0.245776 11.00000 -1.20000
H51B 2 0.743766 0.683289 0.251222 11.00000 -1.20000
AFIX 0
C52 1 0.592809 0.575874 0.123669 11.00000 0.05557 0.05009 =
0.06385 0.03404 0.04022 0.01794
AFIX 23
H52A 2 0.533015 0.554029 0.081320 11.00000 -1.20000
H52B 2 0.640182 0.548422 0.113753 11.00000 -1.20000
AFIX 0
C53 1 0.578654 0.564281 0.186212 11.00000 0.06472 0.04956 =
0.05530 0.02595 0.03390 0.00283
C54 1 0.636533 0.528511 0.227955 11.00000 0.07412 0.08693 =
0.07385 0.05107 0.04943 0.02456
AFIX 43
H54 2 0.688978 0.513783 0.219601 11.00000 -1.20000
AFIX 0
C55 1 0.616852 0.515972 0.278268 11.00000 0.08318 0.09135 =
0.06822 0.04444 0.04712 0.01718
AFIX 43
H55 2 0.654120 0.488645 0.303391 11.00000 -1.20000
AFIX 0
C56 1 0.547127 0.539073 0.297330 11.00000 0.08354 0.07460 =
0.05968 0.04059 0.04439 0.01124
C57 1 0.486865 0.576169 0.258055 11.00000 0.07239 0.07320 =
0.06526 0.04120 0.04174 0.00358
AFIX 43
H57 2 0.435047 0.590833 0.267492 11.00000 -1.20000
AFIX 0
C58 1 0.508208 0.589456 0.205713 11.00000 0.07264 0.05404 =
0.05858 0.03285 0.04247 0.00589
AFIX 43
H58 2 0.472297 0.617860 0.181082 11.00000 -1.20000
AFIX 0
C59 1 0.528517 0.526714 0.358780 11.00000 0.08320 0.06300 =
0.05663 0.03703 0.04272 0.01020
C60 1 0.441919 0.478962 0.343962 11.00000 0.07987 0.06008 =
0.04788 0.03043 0.04220 0.01283
C61 1 0.369848 0.438613 0.277926 11.00000 0.07809 0.08975 =
0.05197 0.03092 0.04306 0.00969
AFIX 43
H61 2 0.369391 0.438575 0.234131 11.00000 -1.20000
AFIX 0
C62 1 0.302193 0.400376 0.287745 11.00000 0.08663 0.07968 =
0.05481 0.02981 0.04818 0.00989
AFIX 43
H62 2 0.242319 0.369946 0.252699 11.00000 -1.20000
AFIX 0
C63 1 0.336187 0.413487 0.361085 11.00000 0.09798 0.08139 =
0.05366 0.02453 0.05067 -0.00339
C64 1 0.691521 0.606537 0.539701 11.00000 0.08400 0.05012 =
0.05895 0.02313 0.04627 0.00976
C65 1 0.743143 0.643022 0.507297 11.00000 0.07988 0.05815 =
0.06070 0.02614 0.04327 0.01060
AFIX 43
H65 2 0.803380 0.678447 0.530798 11.00000 -1.20000
AFIX 0
C66 1 0.688346 0.616449 0.437427 11.00000 0.08306 0.08155 =
0.06212 0.03207 0.04262 0.00108
AFIX 43
H66 2 0.703847 0.629964 0.403098 11.00000 -1.20000
AFIX 0
C67 1 0.603975 0.565076 0.424194 11.00000 0.07196 0.05888 =
0.05776 0.02785 0.04617 0.00923
C68 1 0.276930 0.379607 0.390654 11.00000 0.09374 0.07101 =
0.05568 0.02172 0.05018 -0.00558
C69 1 0.185103 0.325123 0.341745 11.00000 0.09610 0.07481 =
0.05836 0.02603 0.04823 -0.01024
C70 1 0.102849 0.353731 0.323340 11.00000 0.09570 0.07534 =
0.07085 0.02397 0.04593 -0.01016
C71 1 0.020353 0.300840 0.284573 11.00000 0.09934 0.09935 =
0.10861 0.02567 0.03992 -0.01981
AFIX 43
H71 2 -0.035820 0.318706 0.274487 11.00000 -1.20000
AFIX 0
C72 1 0.013763 0.219150 0.258027 11.00000 0.10701 0.09299 =
0.10716 0.02489 0.03870 -0.02285
C73 1 0.086044 0.191987 0.272618 11.00000 0.12231 0.09020 =
0.06758 0.02347 0.04897 -0.01996
AFIX 43
H73 2 0.082165 0.137370 0.254929 11.00000 -1.20000
AFIX 0
C74 1 0.177286 0.250033 0.318876 11.00000 0.11115 0.07359 =
0.06028 0.02484 0.05429 -0.01253
C75 1 0.115648 0.439880 0.355777 11.00000 0.07565 0.08092 =
0.10009 0.02369 0.02816 -0.01449
AFIX 137
H75A 2 0.072331 0.450132 0.379081 11.00000 -1.50000
H75B 2 0.102548 0.462605 0.319118 11.00000 -1.50000
H75C 2 0.180490 0.463607 0.390483 11.00000 -1.50000
AFIX 0
C76 1 -0.077514 0.156869 0.211578 11.00000 0.12211 0.11584 =
0.11327 0.02794 0.03702 -0.03382
AFIX 137
H76A 2 -0.103845 0.161945 0.165537 11.00000 -1.50000
H76B 2 -0.122402 0.163751 0.233794 11.00000 -1.50000
H76C 2 -0.065133 0.104763 0.205461 11.00000 -1.50000
AFIX 0
C77 1 0.261049 0.210928 0.334041 11.00000 0.13062 0.06962 =
0.09207 0.02138 0.05659 -0.00253
AFIX 137
H77A 2 0.308764 0.234530 0.321497 11.00000 -1.50000
H77B 2 0.238966 0.154647 0.306042 11.00000 -1.50000
H77C 2 0.288425 0.218860 0.384179 11.00000 -1.50000
AFIX 0
B1 3 0.219529 0.946138 0.218988 11.00000 0.11788 0.10342 =
0.09090 0.02035 0.06962 0.03834
PART 1
AFIX 6
S3 9 0.205905 0.577081 -0.116260 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O1 6 0.257952 0.653922 -0.102750 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O4 6 0.261496 0.526573 -0.091187 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O5 6 0.119432 0.574578 -0.106454 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
C1A 1 0.163701 0.529730 -0.212629 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F7 4 0.112774 0.456349 -0.236280 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F8 4 0.109631 0.568397 -0.246422 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F9 4 0.234705 0.526162 -0.232976 21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
AFIX 6
PART 0
PART 2
C6A 1 0.197003 0.576512 -0.154100 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
S3A 9 0.103976 0.596264 -0.122398 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O1A 6 0.150359 0.609596 -0.048687 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O4A 6 0.031175 0.524784 -0.163975 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
O5A 6 0.083545 0.664333 -0.138629 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F7A 4 0.167510 0.562340 -0.222861 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F8A 4 0.272383 0.636971 -0.121393 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
F9A 4 0.226273 0.514182 -0.143690 -21.00000 0.11684 0.10340 =
0.27359 0.07517 0.10424 0.05831
AFIX 0
HKLF 4
REM n3560a in P-1
REM R1 = 0.1434 for 5820 Fo > 4sig(Fo) and 0.1940 for all 10661 data
REM 871 parameters refined using 960 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 2.863, deepest hole -1.700, 1-sigma level 0.162
Q1 1 0.1800 0.5963 -0.0507 11.00000 0.05 1.69
Q2 1 0.7262 0.6657 0.0580 11.00000 0.05 1.19
Q3 1 0.7199 0.7415 0.0944 11.00000 0.05 1.03
Q4 1 0.2967 0.8552 0.2609 11.00000 0.05 0.96
Q5 1 0.1207 0.5835 -0.1717 11.00000 0.05 0.92
Q6 1 0.6031 0.6270 0.0012 11.00000 0.05 0.81
Q7 1 0.6031 0.7158 0.0357 11.00000 0.05 0.79
Q8 1 0.6624 0.7066 0.0062 11.00000 0.05 0.74
Q9 1 0.2256 0.5919 -0.2108 11.00000 0.05 0.71
Q10 1 0.8805 0.6843 0.1308 11.00000 0.05 0.70
Q11 1 0.2409 0.9588 0.1779 11.00000 0.05 0.63
Q12 1 -0.0937 0.2734 0.1878 11.00000 0.05 0.59
Q13 1 0.1555 0.9206 0.0697 11.00000 0.05 0.59
Q14 1 0.1419 0.5854 -0.2343 11.00000 0.05 0.58
Q15 1 0.8370 0.5709 -0.0487 11.00000 0.05 0.56
Q16 1 0.1344 0.8053 0.2087 11.00000 0.05 0.56
Q17 1 0.2201 0.9726 0.2882 11.00000 0.05 0.55
Q18 1 0.7593 0.9756 -0.1336 11.00000 0.05 0.54
Q19 1 0.0378 0.8264 -0.0105 11.00000 0.05 0.54
Q20 1 0.4426 0.6743 -0.0314 11.00000 0.05 0.53
;
_shelx_res_checksum 24742
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;
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-15 -2 7 97.56 22.10
-15 -2 8 72.39 19.65
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-15 1 4 48.19 23.40
-15 1 5 105.10 23.60
-15 1 6 204.15 26.60
-15 1 7 189.70 25.20
-15 1 8 29.48 10.25
-15 1 9 7.41 10.09
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-15 1 12 4.08 13.30
-15 1 13 25.21 13.60
-15 2 2 2.20 15.10
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-15 3 5 136.52 24.30
-15 3 6 132.58 23.80
-15 3 7 119.93 22.90
-15 3 8 36.89 15.40
-15 3 9 61.99 25.95
-15 3 10 0.11 10.25
-15 3 11 17.20 14.00
-15 3 12 0.01 13.90
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-15 4 3 328.48 25.80
-15 4 4 355.17 26.90
-15 4 5 118.33 23.60
-15 4 6 0.01 16.00
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-15 4 8 0.93 16.40
-15 4 9 11.81 16.60
-15 4 10 6.58 19.05
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-15 5 2 54.28 15.80
-15 5 3 32.43 16.30
-15 5 4 4.50 16.00
-15 5 5 1.00 16.00
-15 5 6 1.54 16.70
-15 5 7 15.77 17.20
-15 5 8 161.88 24.90
-15 5 9 102.28 23.10
-15 5 10 60.01 10.66
-15 6 2 21.96 15.50
-15 6 3 25.62 15.90
-15 6 4 0.55 16.40
-15 6 5 9.60 17.00
-15 6 6 133.57 24.50
-15 6 7 163.48 23.90
-15 6 8 173.79 24.40
-15 6 9 70.20 22.40
-15 7 4 17.48 17.20
-15 7 5 31.27 17.00
-15 7 6 26.25 17.20
-15 7 7 22.45 16.70
-14 -6 8 153.27 24.40
-14 -6 9 62.91 15.80
-14 -6 10 59.54 14.90
-14 -6 11 17.46 14.00
-14 -6 12 131.47 22.30
-14 -5 5 20.10 15.90
-14 -5 6 164.07 23.54
-14 -5 7 58.47 11.50
-14 -5 8 37.17 14.80
-14 -5 9 14.06 14.10
-14 -5 10 32.46 14.10
-14 -5 11 2.25 13.90
-14 -5 12 55.84 14.10
-14 -5 13 0.76 14.10
-14 -5 14 5.63 14.20
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-14 -4 11 84.78 22.00
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-14 -4 15 25.86 14.20
-14 -3 2 1.30 15.60
-14 -3 3 3.72 15.90
-14 -3 4 3.80 16.10
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-14 -3 6 38.59 10.73
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-14 -3 8 244.09 17.26
-14 -3 9 135.92 21.70
-14 -3 10 57.74 14.30
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-14 -2 8 1.12 9.88
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-14 -2 11 17.95 13.70
-14 -2 12 15.57 13.10
-14 -2 13 64.91 14.30
-14 -2 14 45.05 13.70
-14 -2 15 71.74 14.50
-14 -2 16 65.49 14.50
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-14 -1 2 0.22 16.10
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-14 -1 5 29.75 15.80
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-14 -1 7 112.47 15.96
-14 -1 8 124.28 16.02
-14 -1 9 32.26 10.05
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-14 -1 11 20.89 13.40
-14 -1 12 24.70 13.40
-14 -1 13 5.91 13.40
-14 -1 14 0.06 13.80
-14 -1 15 17.60 13.90
-14 -1 16 160.63 20.30
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-14 0 2 3.84 15.60
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-14 0 11 28.02 13.20
-14 0 12 25.49 14.30
-14 0 13 0.62 13.60
-14 0 14 81.73 20.40
-14 0 15 240.67 21.80
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-14 1 2 72.55 22.70
-14 1 3 73.30 22.10
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-14 1 5 0.04 15.00
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-14 1 9 16.96 10.08
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-14 4 6 17.14 16.10
-14 4 7 1.59 15.60
-14 4 8 83.59 21.55
-14 4 9 91.87 10.85
-14 4 10 119.92 16.90
-14 4 11 20.16 14.30
-14 4 12 35.11 14.50
-14 4 13 11.87 15.00
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-14 5 2 1.60 15.90
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-14 5 4 13.54 16.00
-14 5 5 103.07 24.80
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-14 5 8 7.88 11.13
-14 5 9 33.52 10.58
-14 5 10 19.32 10.90
-14 5 11 5.32 14.60
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-14 6 10 12.37 10.86
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-14 7 8 58.99 17.40
-14 7 9 84.06 22.90
-14 7 10 74.96 11.17
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-14 8 6 56.72 18.20
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-14 8 8 76.39 18.00
-14 8 9 29.90 17.60
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-13 -7 10 21.09 15.00
-13 -7 11 0.20 14.40
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-13 -5 6 0.00 10.49
-13 -5 7 43.40 10.98
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-13 -5 10 8.61 13.60
-13 -5 11 1.38 13.10
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-13 -5 13 0.11 12.20
-13 -5 14 0.05 12.90
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-13 -4 12 1.49 12.00
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-13 -3 6 11.58 9.92
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-13 -3 8 18.69 9.47
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-13 -3 12 0.31 12.30
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-13 2 8 3.32 9.02
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-13 2 10 8.16 9.44
-13 2 11 0.73 12.80
-13 2 12 16.42 12.80
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-13 3 11 5.42 13.20
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-12 6 7 462.87 18.67
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-12 6 11 31.39 14.40
-12 6 12 1.39 13.80
-12 6 13 5.47 14.20
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-12 7 11 58.54 14.90
-12 7 12 45.67 14.90
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-12 8 7 290.61 26.90
-12 8 8 523.43 25.24
-12 8 9 281.43 17.44
-12 8 10 167.83 17.71
-12 8 11 23.80 14.70
-12 8 12 0.47 14.80
-12 8 13 0.02 14.90
-12 9 1 1.47 17.30
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-12 9 6 262.57 28.50
-12 9 7 123.45 27.80
-12 9 8 172.05 17.75
-12 9 9 8.37 11.70
-12 9 10 0.11 27.75
-12 9 11 0.95 15.30
-12 9 12 0.27 15.20
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-12 10 5 9.70 18.10
-12 10 6 7.45 18.70
-12 10 7 83.95 19.90
-12 10 8 105.00 29.00
-12 10 9 46.91 12.81
-12 10 10 7.95 12.36
-12 10 11 1.43 15.40
-12 11 1 1.44 17.60
-12 11 2 0.19 17.90
-12 11 3 0.90 18.00
-12 11 4 0.22 18.50
-12 11 5 50.54 19.80
-12 11 6 164.18 28.90
-12 11 7 297.29 31.60
-12 11 8 152.47 30.90
-12 11 9 80.01 21.00
-12 12 1 0.81 18.40
-12 12 2 0.96 19.10
-12 12 3 11.22 19.20
-12 12 4 34.16 20.40
-12 12 5 170.24 29.10
-12 12 6 93.09 28.50
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-12 13 1 2.05 19.00
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-12 13 3 50.86 20.40
-12 13 4 16.28 20.40
-11 -11 7 131.44 24.30
-11 -11 8 26.61 15.00
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-11 -11 10 5.27 14.30
-11 -11 11 81.28 14.90
-11 -11 12 0.44 13.80
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-11 -11 14 57.17 13.80
-11 -10 4 41.11 11.24
-11 -10 5 141.93 23.40
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-11 -10 7 26.06 15.60
-11 -10 8 9.17 15.10
-11 -10 9 0.03 14.30
-11 -10 10 11.96 13.90
-11 -10 11 32.75 14.30
-11 -10 12 29.82 13.30
-11 -10 13 10.39 13.40
-11 -10 14 189.01 22.00
-11 -10 15 50.64 14.50
-11 -10 16 211.23 24.10
-11 -9 2 2.64 14.90
-11 -9 3 1.47 10.82
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-11 -9 5 0.75 10.96
-11 -9 6 15.78 15.40
-11 -9 7 2.29 14.80
-11 -9 8 10.92 14.50
-11 -9 9 22.99 14.10
-11 -9 10 90.10 22.30
-11 -9 11 42.36 13.30
-11 -9 12 250.72 23.70
-11 -9 13 93.37 20.20
-11 -9 14 128.80 21.20
-11 -9 15 1.36 13.50
-11 -9 16 8.24 13.10
-11 -9 17 48.17 13.30
-11 -8 1 0.00 15.60
-11 -8 2 4.30 15.90
-11 -8 3 0.22 10.82
-11 -8 4 34.89 11.13
-11 -8 5 0.08 10.60
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-11 -8 7 22.75 13.90
-11 -8 8 0.21 13.10
-11 -8 9 10.77 12.80
-11 -8 10 26.38 12.70
-11 -8 11 0.08 11.90
-11 -8 12 34.48 11.90
-11 -8 13 3.07 11.60
-11 -8 14 14.75 12.60
-11 -8 15 276.65 25.10
-11 -8 16 441.81 26.60
-11 -8 17 521.68 27.50
-11 -8 18 62.97 20.80
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-11 -7 2 16.35 16.10
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-11 -7 10 25.32 12.50
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-11 -7 12 36.86 11.40
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-11 -7 15 89.11 20.30
-11 -7 16 8.70 12.30
-11 -7 17 17.71 13.40
-11 -7 18 222.08 20.60
-11 -7 19 9.73 12.40
-11 -6 1 0.02 16.30
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-11 -6 3 1.57 10.15
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-11 -6 5 2.02 9.48
-11 -6 6 1.03 9.40
-11 -6 7 14.53 8.75
-11 -6 8 103.33 19.50
-11 -6 9 237.67 22.90
-11 -6 10 121.17 18.90
-11 -6 11 191.99 20.10
-11 -6 12 6.74 10.70
-11 -6 13 0.47 11.50
-11 -6 14 0.08 11.60
-11 -6 15 98.01 12.30
-11 -6 16 378.90 32.10
-11 -6 17 164.43 21.00
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-11 -5 1 0.60 16.00
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-11 -5 5 2.33 8.88
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-11 -5 8 2.92 8.08
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-11 -5 10 10.02 9.80
-11 -5 11 25.34 17.90
-11 -5 12 122.70 20.00
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-11 -5 14 10.28 11.40
-11 -5 15 78.88 12.90
-11 -5 16 238.33 22.50
-11 -5 17 75.85 13.20
-11 -5 18 266.99 24.80
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-11 -4 1 12.70 15.70
-11 -4 2 2.81 14.80
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-11 -4 6 11.11 7.89
-11 -4 7 59.81 7.73
-11 -4 8 262.98 14.58
-11 -4 9 26.49 9.90
-11 -4 10 185.59 18.90
-11 -4 11 96.78 19.30
-11 -4 12 363.33 24.90
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-11 -4 15 14.02 12.40
-11 -4 16 84.22 20.10
-11 -4 17 24.45 12.70
-11 -4 18 33.20 13.30
-11 -4 19 170.89 20.60
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-11 -3 2 0.26 14.80
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-11 -3 5 11.17 7.49
-11 -3 6 66.89 12.26
-11 -3 7 39.11 9.52
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-11 -3 9 181.05 18.80
-11 -3 10 444.36 25.40
-11 -3 11 59.90 11.70
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-11 -3 13 4.31 10.40
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-11 -3 15 68.49 20.40
-11 -3 16 91.89 12.50
-11 -3 17 352.46 23.90
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-11 -2 12 8.81 10.20
-11 -2 13 437.63 25.90
-11 -2 14 634.14 32.90
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-11 -2 17 76.40 13.40
-11 -2 18 15.83 13.10
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-11 -1 16 20.45 12.40
-11 -1 17 2.53 12.30
-11 -1 18 40.96 20.40
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-11 0 3 0.68 12.00
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-11 0 8 224.93 13.33
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-11 0 12 38.95 11.50
-11 0 13 60.90 11.30
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-11 0 17 228.66 21.50
-11 0 18 115.55 19.80
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-11 1 5 35.56 8.75
-11 1 6 0.01 10.50
-11 1 7 1.27 10.50
-11 1 8 50.24 8.24
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-11 1 10 410.94 16.19
-11 1 11 324.27 22.60
-11 1 12 365.09 22.40
-11 1 13 122.67 20.00
-11 1 14 237.54 21.50
-11 1 15 264.44 19.80
-11 1 16 86.12 20.80
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-11 2 8 783.57 24.76
-11 2 9 591.23 18.80
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-11 2 11 18.84 10.90
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-9 1 11 13.28 8.20
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-9 1 14 143.98 17.80
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-9 2 10 10.95 9.30
-9 2 11 82.02 15.40
-9 2 12 30.81 9.00
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-9 12 8 2.30 11.92
-9 12 9 1.57 22.50
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0 6 12 13.28 12.80
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0 6 14 4.40 15.30
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1 -18 3 15.13 14.60
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1 -1 17 0.85 16.20
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1 0 0 89.82 1.78
1 0 1 298.79 10.90
1 0 2 267.29 5.19
1 0 4 3187.99 160.68
1 0 8 29.01 16.60
1 0 9 32.60 28.60
1 0 10 14.94 19.00
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1 0 12 1.47 10.17
1 0 13 2.45 10.92
1 0 14 54.64 20.68
1 0 15 10.35 15.60
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1 0 17 0.92 15.90
1 0 18 0.06 16.60
1 1 0 61.44 12.10
1 1 1 6940.97 129.17
1 1 2 2282.02 96.02
1 1 3 34.62 17.24
1 1 4 1111.59 165.58
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1 1 6 27.08 24.50
1 1 7 0.04 16.00
1 1 8 65.03 18.10
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1 1 10 19.37 7.46
1 1 11 154.09 13.55
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1 1 13 0.31 11.67
1 1 14 21.70 15.40
1 1 15 17.19 16.70
1 1 16 0.03 17.00
1 1 17 3.79 16.30
1 1 18 14.99 16.80
1 2 0 3065.40 22.45
1 2 1 3504.02 179.16
1 2 2 494.44 23.30
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1 2 4 790.95 28.00
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1 2 8 159.42 10.24
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1 2 10 597.35 20.51
1 2 11 360.95 26.85
1 2 12 374.69 15.31
1 2 13 16.65 9.25
1 2 14 41.52 16.50
1 2 15 8.48 17.40
1 2 16 2.72 17.40
1 2 17 0.09 17.00
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1 3 1 34.29 12.50
1 3 2 92.32 11.99
1 3 3 159.91 29.90
1 3 4 369.22 32.30
1 3 5 187.26 34.30
1 3 6 77.53 51.44
1 3 7 18.47 7.66
1 3 8 535.77 28.43
1 3 9 53.77 8.80
1 3 10 5.85 8.80
1 3 11 127.97 14.40
1 3 12 0.35 11.20
1 3 13 144.92 15.03
1 3 14 8.73 10.44
1 3 15 1.90 18.40
1 4 0 175.76 30.10
1 4 1 65.04 38.15
1 4 2 147.78 22.60
1 4 3 209.59 36.00
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1 4 5 93.34 40.10
1 4 6 86.98 13.73
1 4 7 189.30 13.74
1 4 8 62.41 13.00
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1 4 10 213.53 18.60
1 4 11 1061.73 35.80
1 4 12 218.45 18.60
1 4 13 101.62 19.70
1 4 14 1.34 13.50
1 4 15 21.66 14.80
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1 5 1 16.77 29.90
1 5 2 283.02 33.80
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1 5 4 0.21 26.70
1 5 5 134.88 8.35
1 5 6 5.41 13.00
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1 5 8 168.28 15.00
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1 5 10 129.64 15.60
1 5 11 251.57 20.60
1 5 12 32.72 13.90
1 5 13 1.13 13.90
1 5 14 0.63 14.30
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1 6 1 618.46 44.70
1 6 2 18.70 24.80
1 6 3 49.80 30.60
1 6 4 60.96 20.85
1 6 5 421.68 15.40
1 6 6 73.90 12.60
1 6 7 212.60 14.60
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1 6 10 7.77 11.90
1 6 11 2.11 13.20
1 6 12 45.29 19.10
1 6 13 9.84 14.50
1 6 14 0.28 14.70
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1 7 1 309.24 49.60
1 7 2 41.39 12.43
1 7 3 30.89 13.05
1 7 4 271.00 12.11
1 7 5 125.55 16.50
1 7 6 8.58 8.60
1 7 7 2.33 9.30
1 7 8 34.81 15.20
1 7 9 170.62 17.60
1 7 10 479.59 25.00
1 7 11 135.56 21.10
1 7 12 55.25 14.50
1 7 13 34.55 15.00
1 7 14 0.27 14.50
1 8 0 220.18 35.09
1 8 1 243.06 11.00
1 8 2 2.32 7.31
1 8 3 4.96 6.60
1 8 4 52.14 12.18
1 8 5 106.88 20.65
1 8 6 201.34 17.60
1 8 7 220.02 17.30
1 8 8 541.69 26.70
1 8 9 202.34 19.70
1 8 10 188.74 22.40
1 8 11 104.89 18.90
1 8 12 0.17 14.70
1 8 13 0.01 15.20
1 9 0 2.14 6.38
1 9 1 141.46 11.41
1 9 2 544.22 18.45
1 9 3 481.58 18.49
1 9 4 154.24 19.15
1 9 5 124.46 14.40
1 9 6 155.67 18.10
1 9 7 20.64 12.50
1 9 8 52.90 13.90
1 9 9 10.21 13.90
1 9 10 46.26 14.60
1 9 11 1.19 14.50
1 9 12 7.41 15.00
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1 10 1 90.60 12.46
1 10 2 33.43 7.55
1 10 3 5.33 7.95
1 10 4 0.42 10.80
1 10 5 13.32 9.49
1 10 6 0.16 13.00
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1 10 10 92.74 20.50
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1 11 0 6.60 7.52
1 11 1 0.06 8.90
1 11 2 0.07 8.51
1 11 3 5.29 13.30
1 11 4 21.06 9.87
1 11 5 113.68 21.75
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1 11 7 26.77 14.00
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1 11 10 0.95 14.50
1 12 0 47.06 8.89
1 12 1 114.62 14.29
1 12 2 103.59 24.14
1 12 3 156.23 14.80
1 12 4 1.43 10.24
1 12 5 9.70 10.62
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1 12 7 2.90 13.70
1 12 8 1.64 14.70
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1 13 1 287.83 17.30
1 13 2 76.19 15.44
1 13 3 89.95 16.30
1 13 4 11.45 18.90
1 13 5 8.20 14.80
1 13 6 18.31 15.10
1 13 7 9.74 14.30
1 14 0 141.40 23.50
1 14 1 67.41 16.10
1 14 2 131.76 21.45
1 14 3 10.52 11.15
1 14 4 61.07 11.43
1 14 5 4.15 14.50
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1 15 1 69.51 23.30
1 15 2 118.43 23.70
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1 16 1 0.12 15.80
2 -18 2 92.48 21.50
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2 -9 3 185.18 17.60
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2 -9 7 59.21 10.40
2 -9 8 37.49 10.10
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2 -9 10 61.05 7.28
2 -9 11 11.99 7.89
2 -9 12 1.99 8.25
2 -9 13 50.62 14.38
2 -9 14 6.18 12.77
2 -9 15 21.19 11.11
2 -9 16 27.05 15.44
2 -9 17 0.12 15.80
2 -9 18 0.51 16.30
2 -9 19 66.19 26.90
2 -8 0 279.95 44.80
2 -8 1 308.06 37.30
2 -8 2 320.66 39.30
2 -8 7 13.84 10.40
2 -8 8 2.88 6.34
2 -8 9 53.09 6.49
2 -8 10 114.13 32.20
2 -8 11 353.10 15.52
2 -8 12 227.65 14.62
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2 -8 14 48.20 9.45
2 -8 15 24.87 11.77
2 -8 16 28.86 13.66
2 -8 17 0.13 17.75
2 -8 18 0.00 15.30
2 -8 19 4.89 15.20
2 -7 0 1322.06 83.29
2 -7 1 176.80 28.80
2 -7 2 256.45 41.00
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2 -7 8 120.76 21.60
2 -7 9 18.31 6.75
2 -7 10 15.74 6.85
2 -7 11 691.30 26.37
2 -7 12 191.81 13.39
2 -7 13 90.21 10.88
2 -7 14 16.73 8.82
2 -7 15 48.78 12.64
2 -7 16 10.64 13.23
2 -7 17 73.17 13.88
2 -7 18 85.34 26.10
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2 -6 0 939.95 44.19
2 -6 1 829.12 53.99
2 -6 2 150.65 17.76
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2 -6 9 475.65 17.97
2 -6 10 28.10 6.90
2 -6 11 110.77 12.42
2 -6 12 101.29 15.42
2 -6 13 74.29 8.45
2 -6 14 172.30 23.74
2 -6 15 0.02 12.24
2 -6 16 13.92 12.89
2 -6 17 90.62 39.64
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2 -5 0 9.30 11.32
2 -5 1 3823.39 121.32
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2 -5 3 42.80 14.30
2 -5 9 169.08 15.30
2 -5 10 718.85 24.43
2 -5 11 522.05 26.20
2 -5 12 935.64 25.96
2 -5 13 263.56 28.50
2 -5 14 124.19 20.18
2 -5 15 0.00 12.54
2 -5 16 8.63 13.10
2 -5 17 12.55 15.05
2 -5 18 6.75 13.11
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2 -4 1 1727.27 100.33
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2 -4 11 674.55 21.77
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2 -4 13 4.33 11.90
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2 -3 1 628.95 30.86
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2 -3 8 3.87 17.10
2 -3 9 68.69 13.30
2 -3 10 22.24 9.30
2 -3 11 56.26 27.30
2 -3 12 23.09 9.90
2 -3 13 99.53 24.80
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2 -3 16 0.44 13.22
2 -3 17 0.07 14.05
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2 -2 0 2509.76 178.38
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2 -2 8 60.17 27.20
2 -2 9 645.66 18.18
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2 -2 11 982.67 30.58
2 -2 12 300.01 20.14
2 -2 13 337.43 21.18
2 -2 14 0.94 16.20
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2 -2 17 3.50 16.60
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2 -1 0 342.39 8.47
2 -1 1 1.59 5.29
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2 -1 8 42.01 18.20
2 -1 9 808.71 71.09
2 -1 10 625.10 28.45
2 -1 11 397.79 19.22
2 -1 12 7.89 10.63
2 -1 13 27.80 11.47
2 -1 14 102.71 13.12
2 -1 15 1.53 15.40
2 -1 16 35.93 23.70
2 -1 18 0.04 16.80
2 0 0 47.55 14.20
2 0 1 177.66 12.50
2 0 2 227.44 36.45
2 0 3 199.02 31.09
2 0 7 261.32 28.70
2 0 8 110.60 18.60
2 0 9 157.16 22.24
2 0 10 0.00 9.54
2 0 11 39.61 10.12
2 0 12 245.04 49.44
2 0 13 4.35 12.23
2 0 14 28.76 13.44
2 0 15 1.30 15.80
2 0 16 20.26 16.70
2 0 17 0.15 17.00
2 1 0 537.57 11.28
2 1 1 1491.12 80.24
2 1 2 246.48 20.30
2 1 3 136.36 16.97
2 1 4 62.64 20.50
2 1 5 36.38 22.00
2 1 6 217.05 21.23
2 1 7 41.47 27.20
2 1 8 484.89 40.20
2 1 9 289.47 16.73
2 1 10 502.87 17.49
2 1 11 336.52 12.63
2 1 12 370.19 27.35
2 1 13 5.61 13.45
2 1 14 13.00 16.90
2 1 15 7.82 16.50
2 2 0 615.81 42.40
2 2 1 644.43 19.65
2 2 2 103.56 28.04
2 2 3 0.41 19.50
2 2 4 135.98 31.90
2 2 5 40.88 22.90
2 2 6 1115.92 58.82
2 2 7 52.49 12.45
2 2 8 381.22 22.36
2 2 9 296.07 17.80
2 2 10 328.38 23.54
2 2 11 40.27 10.23
2 2 12 44.73 8.86
2 2 13 13.63 12.50
2 3 0 166.33 22.65
2 3 1 1544.03 66.85
2 3 2 63.18 33.80
2 3 3 483.76 37.60
2 3 4 208.10 26.40
2 3 5 47.92 15.48
2 3 6 95.90 10.27
2 3 7 18.10 10.87
2 3 8 7.69 26.04
2 3 9 119.44 13.79
2 3 10 19.43 10.70
2 3 11 526.59 22.90
2 3 12 95.15 17.90
2 3 13 69.59 13.50
2 3 14 0.64 14.10
2 4 0 19.27 12.19
2 4 1 764.44 80.19
2 4 2 179.89 38.00
2 4 3 37.60 25.10
2 4 4 0.70 26.60
2 4 5 170.99 11.20
2 4 6 7.67 30.40
2 4 7 329.22 14.40
2 4 8 315.09 17.00
2 4 9 968.32 38.20
2 4 10 274.63 19.70
2 4 11 259.66 20.30
2 4 12 0.47 13.00
2 4 13 0.62 14.30
2 4 14 1.20 14.10
2 5 0 317.01 37.70
2 5 1 2386.82 64.69
2 5 2 43.62 36.80
2 5 3 37.59 29.30
2 5 4 330.24 11.42
2 5 5 131.90 16.94
2 5 6 0.01 8.20
2 5 7 181.21 15.60
2 5 8 132.56 16.40
2 5 9 182.77 16.10
2 5 10 11.10 12.70
2 5 11 5.27 12.80
2 5 12 11.69 14.50
2 5 13 2.48 15.10
2 5 14 0.48 14.20
2 6 0 486.50 41.80
2 6 1 279.49 44.70
2 6 2 0.11 10.10
2 6 3 139.81 21.40
2 6 4 360.98 15.86
2 6 5 156.98 13.10
2 6 6 78.93 14.50
2 6 7 15.76 9.70
2 6 8 110.86 16.80
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2 6 10 176.63 19.10
2 6 11 107.60 19.00
2 6 12 1.05 15.00
2 6 13 0.00 15.00
2 6 14 0.45 14.60
2 7 0 77.77 28.10
2 7 1 200.86 10.78
2 7 2 45.10 6.87
2 7 3 17.39 7.04
2 7 4 3.41 8.15
2 7 5 14.27 9.20
2 7 6 248.33 17.00
2 7 7 195.91 18.70
2 7 8 162.18 18.80
2 7 9 27.73 12.50
2 7 10 36.91 18.90
2 7 11 53.18 14.80
2 7 12 0.01 15.00
2 7 13 3.11 14.60
2 8 0 85.95 16.83
2 8 1 96.19 10.92
2 8 2 312.01 14.14
2 8 3 100.92 12.39
2 8 4 91.08 12.68
2 8 5 81.89 11.00
2 8 6 166.88 18.30
2 8 7 1.59 11.80
2 8 8 48.33 12.70
2 8 9 14.87 13.60
2 8 10 20.15 14.50
2 8 11 6.09 15.20
2 8 12 0.01 14.60
2 9 0 267.02 13.49
2 9 1 425.01 15.48
2 9 2 246.46 22.50
2 9 3 119.37 13.48
2 9 4 12.60 8.90
2 9 5 71.81 11.40
2 9 6 4.23 11.70
2 9 7 36.47 12.80
2 9 8 75.04 18.00
2 9 9 58.16 14.30
2 9 10 15.94 15.20
2 9 11 37.77 14.90
2 10 0 55.41 11.91
2 10 1 41.56 7.96
2 10 2 1.34 7.94
2 10 3 109.61 13.26
2 10 4 18.38 12.30
2 10 5 223.06 19.60
2 10 6 18.72 13.30
2 10 8 38.43 14.50
2 10 9 30.63 14.80
2 10 10 0.34 14.30
2 11 0 217.91 15.37
2 11 1 98.59 14.10
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2 11 3 413.74 21.26
2 11 4 13.83 10.26
2 11 5 8.91 13.50
2 11 6 0.08 14.00
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2 11 8 9.28 14.40
2 11 9 2.28 14.00
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2 12 2 1.43 10.39
2 12 3 93.69 10.89
2 12 4 22.30 11.14
2 12 5 14.03 14.50
2 12 6 3.14 14.30
2 12 7 0.29 13.90
2 12 8 11.38 14.10
2 13 0 45.22 14.70
2 13 1 0.52 16.35
2 13 2 137.07 18.25
2 13 3 33.57 11.48
2 13 4 63.53 28.40
2 13 5 0.18 14.40
2 13 6 0.24 14.30
2 14 0 208.26 25.80
2 14 1 130.97 20.25
2 14 2 212.86 18.10
2 14 3 10.81 19.75
2 14 4 42.40 20.70
2 15 0 42.49 16.00
2 15 1 0.29 16.50
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2 16 0 29.72 16.00
3 -18 2 0.14 14.80
3 -18 3 28.12 14.70
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3 -18 6 1.16 12.70
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3 -17 3 123.11 21.90
3 -17 4 80.72 20.90
3 -17 5 87.05 20.30
3 -17 6 2.87 12.00
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3 -16 0 47.39 16.50
3 -16 1 138.64 24.10
3 -16 2 154.08 23.00
3 -16 3 258.91 23.80
3 -16 4 66.17 21.40
3 -16 5 21.65 12.70
3 -16 6 4.40 12.00
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3 -15 0 9.68 15.90
3 -15 1 12.40 15.40
3 -15 2 0.05 14.60
3 -15 3 18.61 13.80
3 -15 4 109.62 21.10
3 -15 5 2.69 11.90
3 -15 6 0.01 11.40
3 -15 7 0.09 10.60
3 -14 0 551.84 30.10
3 -14 1 524.96 30.60
3 -14 2 547.48 27.00
3 -14 3 154.42 24.00
3 -14 4 70.20 12.30
3 -14 5 3.62 11.20
3 -14 6 0.27 10.50
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3 -13 0 532.68 33.20
3 -13 1 425.09 26.90
3 -13 2 178.52 22.40
3 -13 3 4.04 11.90
3 -13 4 1.47 11.50
3 -13 5 0.83 11.30
3 -13 6 2.90 10.90
3 -13 7 1.46 9.90
3 -13 14 41.66 29.50
3 -13 15 42.00 31.40
3 -12 0 103.90 21.90
3 -12 1 2.29 11.90
3 -12 2 46.77 11.50
3 -12 3 140.72 18.70
3 -12 4 37.06 10.80
3 -12 5 136.78 17.60
3 -12 6 36.15 16.60
3 -12 7 98.50 17.40
3 -12 12 165.12 34.30
3 -12 13 116.56 34.50
3 -12 14 112.19 16.24
3 -12 15 32.41 21.04
3 -12 16 1.02 18.90
3 -12 17 0.09 18.30
3 -11 0 613.18 32.90
3 -11 1 816.31 32.60
3 -11 2 453.47 23.40
3 -11 3 615.56 29.50
3 -11 4 191.64 18.00
3 -11 5 187.15 17.10
3 -11 6 24.83 8.70
3 -11 9 87.34 27.00
3 -11 10 272.91 30.90
3 -11 11 266.51 31.70
3 -11 12 432.60 35.40
3 -11 13 298.37 34.60
3 -11 14 180.99 25.43
3 -11 15 23.66 15.73
3 -11 16 1.29 15.62
3 -11 17 0.02 17.20
3 -10 0 250.23 20.80
3 -10 1 85.61 10.90
3 -10 2 3.44 9.70
3 -10 3 14.73 9.10
3 -10 4 20.87 9.00
3 -10 5 93.61 15.20
3 -10 6 12.38 8.20
3 -10 8 266.94 24.80
3 -10 9 152.89 27.00
3 -10 10 132.05 27.20
3 -10 11 25.65 14.80
3 -10 12 20.23 9.95
3 -10 13 1.06 9.79
3 -10 14 8.67 11.30
3 -10 15 1.41 10.82
3 -10 16 34.17 22.14
3 -10 17 3.92 31.45
3 -10 18 1.57 16.30
3 -9 0 69.11 9.17
3 -9 1 66.90 15.90
3 -9 2 829.52 29.70
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3 -9 4 85.50 13.20
3 -9 5 18.75 7.60
3 -9 6 12.79 10.60
3 -9 7 14.15 11.00
3 -9 8 56.84 23.10
3 -9 9 6.49 11.90
3 -9 10 2.91 8.40
3 -9 11 350.03 34.55
3 -9 12 300.11 19.44
3 -9 13 301.07 18.05
3 -9 14 73.91 10.22
3 -9 15 44.40 14.61
3 -9 16 66.93 35.49
3 -9 17 0.10 34.40
3 -9 18 1.54 15.80
3 -8 0 602.92 18.90
3 -8 1 196.15 42.90
3 -8 2 822.83 51.19
3 -8 5 283.15 22.80
3 -8 6 0.72 10.20
3 -8 7 55.10 21.90
3 -8 8 28.49 8.30
3 -8 9 238.24 14.23
3 -8 10 207.46 13.59
3 -8 11 966.60 29.14
3 -8 12 402.41 16.25
3 -8 13 184.95 19.62
3 -8 14 0.01 9.62
3 -8 15 7.72 13.50
3 -8 16 2.72 16.70
3 -8 17 31.87 28.40
3 -8 18 51.26 39.80
3 -7 0 2048.24 121.24
3 -7 1 21.23 14.15
3 -7 2 753.40 47.30
3 -7 3 128.32 28.20
3 -7 7 38.60 10.20
3 -7 8 29.00 12.68
3 -7 9 533.20 16.99
3 -7 10 7.94 7.15
3 -7 11 40.16 7.77
3 -7 12 2.14 11.15
3 -7 13 12.07 9.73
3 -7 14 84.89 50.79
3 -7 15 4.01 13.34
3 -7 16 12.28 13.67
3 -7 17 7.93 42.30
3 -7 18 41.17 34.70
3 -6 0 178.73 12.40
3 -6 1 2614.51 157.09
3 -6 2 0.94 10.27
3 -6 3 11.39 16.00
3 -6 8 208.96 24.70
3 -6 9 0.20 6.70
3 -6 10 294.68 21.16
3 -6 11 394.76 17.79
3 -6 12 602.52 21.07
3 -6 13 49.55 11.79
3 -6 14 48.03 18.68
3 -6 15 26.46 13.56
3 -6 16 3.67 13.51
3 -6 17 10.89 15.65
3 -6 18 0.82 27.95
3 -5 0 33.72 22.69
3 -5 1 2372.54 76.25
3 -5 2 155.05 9.94
3 -5 3 259.49 33.10
3 -5 8 468.71 27.30
3 -5 9 130.65 11.79
3 -5 10 693.63 20.30
3 -5 11 270.77 19.10
3 -5 12 79.04 11.27
3 -5 13 42.49 12.65
3 -5 14 9.40 12.53
3 -5 15 0.40 13.09
3 -5 16 4.98 13.61
3 -5 17 0.05 13.04
3 -5 18 0.04 13.25
3 -4 0 624.24 36.79
3 -4 1 106.84 28.44
3 -4 2 497.05 32.95
3 -4 8 163.92 41.50
3 -4 9 21.48 12.55
3 -4 10 28.30 11.50
3 -4 11 169.47 23.50
3 -4 12 72.95 11.77
3 -4 13 128.40 29.10
3 -4 14 15.75 13.14
3 -4 15 0.18 13.53
3 -4 16 7.99 13.31
3 -4 17 0.37 13.21
3 -4 18 0.02 14.40
3 -3 0 1669.24 88.88
3 -3 1 35.88 16.21
3 -3 2 81.56 8.87
3 -3 7 178.59 27.00
3 -3 8 17.30 20.00
3 -3 9 847.40 31.55
3 -3 10 1264.08 40.39
3 -3 11 1010.34 38.90
3 -3 12 192.52 19.40
3 -3 13 98.19 21.00
3 -3 14 0.37 13.18
3 -3 15 0.54 13.66
3 -3 16 12.23 14.13
3 -3 17 0.64 14.35
3 -3 18 0.12 14.90
3 -2 0 7256.84 212.82
3 -2 1 178.88 16.01
3 -2 2 594.69 33.95
3 -2 6 525.87 42.80
3 -2 7 541.73 34.90
3 -2 8 126.18 27.80
3 -2 9 225.64 16.92
3 -2 10 277.37 20.40
3 -2 11 100.70 13.70
3 -2 12 1.01 14.70
3 -2 13 47.30 12.58
3 -2 14 5.02 13.29
3 -2 15 0.12 13.95
3 -2 16 26.30 23.94
3 -2 17 0.04 16.20
3 -1 0 588.12 46.27
3 -1 1 567.16 21.84
3 -1 2 2322.67 68.89
3 -1 3 3204.38 149.59
3 -1 6 91.88 16.50
3 -1 7 5.48 17.40
3 -1 8 519.95 39.50
3 -1 9 152.97 16.47
3 -1 10 116.91 18.30
3 -1 11 9.83 10.41
3 -1 12 21.57 11.55
3 -1 13 33.16 12.40
3 -1 14 1.05 12.91
3 -1 15 0.33 18.05
3 -1 16 15.40 17.40
3 0 1 1355.66 57.58
3 0 2 1339.01 34.62
3 0 3 429.79 21.66
3 0 4 112.47 30.70
3 0 6 660.77 49.70
3 0 7 41.27 19.00
3 0 8 541.11 30.65
3 0 9 656.08 17.47
3 0 10 642.18 31.00
3 0 11 82.38 11.05
3 0 12 228.99 33.75
3 0 13 7.97 12.66
3 0 14 20.92 13.32
3 1 0 102.15 10.70
3 1 1 88.65 14.60
3 1 2 2.40 16.80
3 1 3 133.01 20.60
3 1 4 363.31 35.60
3 1 5 35.76 14.87
3 1 6 676.35 29.60
3 1 7 13.11 15.15
3 1 8 422.79 18.03
3 1 9 284.48 14.71
3 1 10 350.94 27.00
3 1 11 3.29 9.55
3 1 12 6.77 29.60
3 1 13 36.46 29.30
3 2 0 141.31 32.00
3 2 1 473.76 32.50
3 2 2 2506.05 109.59
3 2 3 1909.61 96.29
3 2 4 1165.41 59.99
3 2 5 32.11 15.13
3 2 6 17.42 7.93
3 2 7 15.40 7.41
3 2 8 1.08 8.80
3 2 9 87.14 19.65
3 2 10 0.11 9.54
3 2 11 280.57 16.58
3 2 12 52.64 16.10
3 3 0 1777.36 61.69
3 3 1 323.76 39.50
3 3 2 1248.80 62.19
3 3 3 403.81 39.90
3 3 4 165.34 23.85
3 3 5 37.45 8.01
3 3 6 124.14 12.91
3 3 7 422.97 16.81
3 3 8 48.89 24.40
3 3 9 283.99 19.74
3 3 10 242.60 17.00
3 3 11 130.06 19.30
3 3 12 1.12 13.10
3 3 13 0.32 13.60
3 4 0 1051.49 114.09
3 4 1 1356.19 45.80
3 4 2 16.36 30.30
3 4 3 202.54 44.74
3 4 4 670.07 19.70
3 4 5 309.01 46.74
3 4 6 29.73 30.50
3 4 7 50.20 13.90
3 4 8 70.27 14.30
3 4 9 68.21 11.10
3 4 10 0.02 12.20
3 4 11 5.92 13.50
3 4 12 7.43 13.90
3 4 13 0.11 14.30
3 4 14 2.42 14.40
3 5 0 393.16 25.60
3 5 1 703.53 54.49
3 5 2 452.15 54.09
3 5 3 375.53 13.79
3 5 4 352.71 29.00
3 5 5 83.21 9.20
3 5 6 51.17 9.40
3 5 7 23.54 9.70
3 5 8 92.97 15.30
3 5 9 141.99 20.30
3 5 10 34.52 13.40
3 5 11 1.37 14.70
3 5 12 0.00 14.70
3 5 13 2.00 15.20
3 5 14 2.72 14.30
3 6 0 832.88 60.99
3 6 1 192.10 20.94
3 6 2 8.27 14.92
3 6 3 180.90 11.40
3 6 4 362.95 20.50
3 6 5 86.11 15.20
3 6 6 205.24 16.90
3 6 7 19.39 10.50
3 6 8 28.76 11.80
3 6 9 4.51 12.90
3 6 10 8.51 14.60
3 6 11 50.22 15.30
3 6 12 0.49 15.30
3 6 13 0.38 15.00
3 7 0 23.28 6.67
3 7 1 252.26 19.91
3 7 2 409.05 16.74
3 7 3 36.46 7.52
3 7 4 51.12 11.82
3 7 5 1.86 9.80
3 7 6 4.33 10.90
3 7 7 61.30 16.90
3 7 8 1.44 12.70
3 7 9 36.48 14.50
3 7 10 11.59 15.00
3 7 11 18.59 15.40
3 7 12 0.09 15.40
3 8 0 346.94 23.05
3 8 1 283.94 21.95
3 8 2 329.02 16.44
3 8 3 0.11 7.88
3 8 4 7.72 8.32
3 8 5 225.36 18.20
3 8 6 0.48 11.80
3 8 7 13.24 12.70
3 8 8 13.58 14.20
3 8 9 35.10 14.80
3 8 10 5.52 14.60
3 8 11 23.17 15.80
3 9 0 159.38 12.64
3 9 1 107.01 12.58
3 9 2 8.66 8.12
3 9 3 316.37 16.46
3 9 4 13.08 12.70
3 9 5 50.31 12.70
3 9 6 0.99 13.10
3 9 7 0.02 13.60
3 9 8 8.81 13.90
3 9 9 62.22 14.70
3 9 10 0.65 14.90
3 10 0 8.18 8.06
3 10 1 183.65 15.00
3 10 2 155.60 22.40
3 10 3 1186.32 54.50
3 10 4 134.18 16.55
3 10 5 0.46 13.50
3 10 6 23.94 13.90
3 10 7 0.73 13.90
3 10 8 3.12 14.30
3 10 9 0.19 14.80
3 11 0 238.69 16.47
3 11 1 663.25 20.04
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3 13 5 0.00 14.60
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4 -18 2 45.67 15.00
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4 -15 14 30.02 30.40
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4 0 2 94.51 20.90
4 0 3 0.10 14.57
4 0 4 359.86 40.80
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4 0 6 148.65 29.80
4 0 7 0.17 15.70
4 0 8 81.31 12.13
4 0 9 71.97 8.35
4 0 10 256.44 37.40
4 0 11 1.08 26.00
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4 0 14 10.04 30.30
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4 1 1 178.61 19.41
4 1 2 2758.95 217.68
4 1 3 1333.16 118.44
4 1 4 418.68 22.41
4 1 5 19.92 15.29
4 1 6 1.55 8.37
4 1 7 79.67 12.75
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4 1 9 51.09 14.15
4 1 10 0.12 15.50
4 1 11 17.46 10.25
4 1 12 0.14 31.20
4 1 13 3.87 30.40
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4 2 1 391.58 33.30
4 2 2 1682.75 118.09
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4 2 4 6.85 15.09
4 2 5 17.79 10.21
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4 2 7 158.85 13.85
4 2 8 49.25 17.85
4 2 9 184.85 28.00
4 2 10 63.22 16.70
4 2 11 26.34 23.69
4 2 12 9.08 12.40
4 3 0 247.95 32.80
4 3 1 76.48 34.20
4 3 2 72.89 29.60
4 3 3 17.73 23.58
4 3 4 446.63 13.01
4 3 5 139.92 14.61
4 3 6 29.79 9.02
4 3 7 58.80 17.65
4 3 8 150.96 19.60
4 3 9 82.54 31.45
4 3 10 11.88 12.40
4 3 11 16.25 13.60
4 3 12 0.60 13.70
4 3 13 1.13 14.00
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4 6 1 279.37 14.14
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4 6 4 215.49 18.00
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4 6 7 0.61 12.00
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4 7 10 1.44 15.60
4 7 11 65.58 20.60
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4 9 6 6.78 13.90
4 9 7 0.21 14.40
4 9 8 0.29 14.90
4 9 9 1.71 14.80
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5 3 1 1208.54 86.99
5 3 2 1544.91 67.79
5 3 3 579.25 23.94
5 3 4 17.69 9.75
5 3 5 94.75 14.45
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5 3 8 20.84 21.85
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5 4 7 10.50 11.90
5 4 8 24.71 12.90
5 4 9 10.60 14.10
5 4 10 49.21 14.90
5 4 11 17.24 15.20
5 4 12 14.95 14.50
5 4 13 0.64 14.30
5 5 0 177.89 11.51
5 5 1 78.82 11.20
5 5 2 425.22 14.20
5 5 3 140.90 16.20
5 5 4 229.37 21.20
5 5 5 0.81 10.90
5 5 6 8.78 11.60
5 5 7 4.06 12.80
5 5 8 12.14 13.90
5 5 9 2.70 14.70
5 5 10 50.31 15.90
5 5 11 0.94 15.00
5 5 12 8.67 14.40
5 6 0 1153.41 34.93
5 6 1 636.94 23.41
5 6 2 867.05 26.60
5 6 3 14.47 10.90
5 6 4 19.36 11.10
5 6 5 11.71 11.90
5 6 6 7.25 12.80
5 6 7 0.13 13.70
5 6 8 2.06 14.80
5 6 9 23.86 15.70
5 6 10 5.61 15.60
5 6 11 104.64 20.00
5 7 0 1051.53 22.10
5 7 1 305.73 19.00
5 7 2 245.85 14.30
5 7 3 110.16 17.30
5 7 4 1.83 12.30
5 7 5 9.33 13.20
5 7 6 1.20 13.80
5 7 7 3.77 14.50
5 7 8 22.92 15.00
5 7 9 81.43 20.80
5 7 10 0.49 15.10
5 8 0 18.66 7.98
5 8 1 129.84 12.90
5 8 2 12.45 9.03
5 8 3 165.34 20.00
5 8 4 0.69 13.20
5 8 5 1.31 13.70
5 8 6 2.83 14.20
5 8 7 0.54 14.60
5 8 8 1.15 15.10
5 8 9 1.27 15.20
5 9 0 197.27 13.85
5 9 1 333.53 19.64
5 9 2 11.69 9.63
5 9 3 101.43 19.40
5 9 4 29.60 14.20
5 9 5 4.01 14.70
5 9 6 3.36 14.60
5 9 7 0.02 14.70
5 9 8 0.04 14.80
5 10 0 54.90 9.62
5 10 1 24.66 10.09
5 10 2 3.46 10.41
5 10 3 16.45 15.20
5 10 4 125.93 22.60
5 10 5 6.46 14.70
5 10 6 4.15 14.50
5 10 7 1.80 14.50
5 11 0 49.65 10.39
5 11 1 39.44 11.13
5 11 2 183.08 16.74
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5 11 5 0.01 14.60
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5 12 0 80.66 11.03
5 12 1 1.78 11.06
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5 12 3 49.47 15.50
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5 13 0 12.07 10.85
5 13 1 94.37 14.43
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6 -17 0 0.53 15.80
6 -17 1 0.02 15.30
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6 -16 6 14.69 13.10
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6 -14 0 0.10 17.10
6 -14 1 0.01 16.40
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6 -13 0 0.08 15.30
6 -13 1 2.47 14.90
6 -13 2 0.77 14.40
6 -13 3 56.07 14.30
6 -13 4 6.79 13.40
6 -13 5 14.58 13.00
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6 -13 13 33.46 32.60
6 -13 14 20.12 32.80
6 -12 0 38.82 14.10
6 -12 1 0.33 12.70
6 -12 2 49.14 12.50
6 -12 3 44.13 20.00
6 -12 4 87.54 19.10
6 -12 5 37.58 11.90
6 -12 6 83.39 18.40
6 -12 12 0.76 31.20
6 -12 13 26.90 31.90
6 -12 14 12.48 33.10
6 -11 0 356.21 29.80
6 -11 1 193.72 19.10
6 -11 2 514.07 28.60
6 -11 3 284.14 19.40
6 -11 4 173.97 18.30
6 -11 5 8.30 10.50
6 -11 12 45.02 30.80
6 -11 13 116.20 34.70
6 -11 14 7.83 33.10
6 -11 15 10.57 32.00
6 -10 0 452.18 22.90
6 -10 1 98.92 18.00
6 -10 2 129.29 19.20
6 -10 3 0.95 15.60
6 -10 4 16.22 15.70
6 -10 5 22.53 15.40
6 -10 11 24.55 28.80
6 -10 12 4.40 14.70
6 -10 13 1.07 12.89
6 -10 14 2.27 32.60
6 -10 15 6.20 33.10
6 -9 0 106.40 15.90
6 -9 1 107.02 15.70
6 -9 2 75.94 17.10
6 -9 3 478.14 17.50
6 -9 4 469.77 26.90
6 -9 5 573.19 25.00
6 -9 9 19.34 13.40
6 -9 10 6.11 13.80
6 -9 11 0.03 11.09
6 -9 12 37.85 11.29
6 -9 13 2.32 10.76
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6 -9 15 0.52 12.44
6 -8 0 196.01 17.90
6 -8 1 354.86 19.60
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6 -8 5 51.42 8.70
6 -8 7 3.45 12.00
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6 -8 9 16.01 12.30
6 -8 10 11.69 10.45
6 -8 11 10.21 10.40
6 -8 12 2.54 8.63
6 -8 13 7.48 11.72
6 -8 14 21.12 17.50
6 -8 15 0.41 11.69
6 -7 0 7.32 7.70
6 -7 1 0.22 8.30
6 -7 2 33.70 9.20
6 -7 3 0.54 9.00
6 -7 4 308.16 19.90
6 -7 5 141.32 17.50
6 -7 6 239.69 22.70
6 -7 7 64.49 12.30
6 -7 8 103.83 23.60
6 -7 9 72.49 18.75
6 -7 10 27.69 12.43
6 -7 11 0.72 21.00
6 -7 12 0.57 21.95
6 -7 13 8.79 32.30
6 -7 14 2.13 11.20
6 -7 15 13.84 11.74
6 -6 0 118.17 16.42
6 -6 1 33.06 15.50
6 -6 2 530.24 24.20
6 -6 3 138.69 22.09
6 -6 4 53.51 8.70
6 -6 5 37.44 6.85
6 -6 6 188.68 22.90
6 -6 7 26.26 11.10
6 -6 8 9.75 10.46
6 -6 9 0.77 11.27
6 -6 10 5.45 12.20
6 -6 11 13.86 32.50
6 -6 12 22.25 14.57
6 -6 13 37.74 15.23
6 -6 14 6.54 15.23
6 -6 15 5.51 15.04
6 -5 0 649.03 47.40
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6 -5 4 2.14 10.50
6 -5 5 7.04 14.30
6 -5 6 35.86 10.70
6 -5 7 131.05 11.75
6 -5 8 12.73 31.34
6 -5 9 10.50 11.46
6 -5 10 4.99 12.20
6 -5 11 38.36 13.68
6 -5 12 0.97 15.65
6 -5 13 0.95 14.70
6 -5 14 2.79 15.67
6 -5 15 9.87 31.90
6 -4 0 1074.16 81.39
6 -4 1 27.40 23.90
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6 -4 3 274.39 40.20
6 -4 5 403.37 23.40
6 -4 6 116.37 15.43
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6 -4 8 3.11 14.65
6 -4 9 0.03 11.05
6 -4 10 23.38 12.19
6 -4 11 0.22 13.03
6 -4 12 1.13 30.50
6 -4 13 0.12 32.50
6 -4 14 16.08 32.30
6 -4 15 26.84 29.40
6 -3 0 166.43 23.08
6 -3 1 285.64 22.08
6 -3 2 684.70 69.79
6 -3 3 1407.40 64.29
6 -3 5 7.53 7.99
6 -3 6 119.69 31.45
6 -3 7 0.25 20.80
6 -3 8 10.40 23.00
6 -3 9 6.15 24.10
6 -3 10 20.80 26.90
6 -3 11 12.72 29.50
6 -3 12 0.11 31.60
6 -3 13 10.83 31.80
6 -3 14 1.02 29.80
6 -3 15 0.23 30.90
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6 -2 1 708.64 41.80
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6 -2 7 4.59 12.70
6 -2 8 0.00 22.80
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6 -2 10 3.97 27.60
6 -2 11 0.55 30.40
6 -2 12 2.89 31.00
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6 -2 14 0.44 31.90
6 -2 15 4.63 30.40
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6 -1 1 1015.31 57.19
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6 -1 5 4.77 12.48
6 -1 6 66.83 11.62
6 -1 7 0.03 8.60
6 -1 8 0.18 8.20
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6 -1 10 1.48 28.90
6 -1 11 8.08 29.90
6 -1 12 45.46 30.70
6 -1 13 5.57 33.30
6 -1 14 3.90 31.60
6 0 0 957.64 79.89
6 0 1 1748.72 90.89
6 0 2 872.56 35.22
6 0 3 316.08 17.33
6 0 4 72.73 10.09
6 0 5 50.37 8.42
6 0 6 7.27 15.45
6 0 7 10.78 8.60
6 0 8 2.09 12.30
6 0 9 8.44 10.00
6 0 10 32.38 22.60
6 0 11 54.25 33.30
6 0 12 81.68 34.60
6 0 13 64.85 32.60
6 1 0 229.71 38.50
6 1 1 79.53 27.90
6 1 2 0.36 8.25
6 1 3 0.76 10.65
6 1 4 0.16 14.60
6 1 5 205.39 12.82
6 1 6 46.55 15.90
6 1 7 4.02 8.95
6 1 8 1.87 9.63
6 1 9 0.18 14.80
6 1 10 0.07 11.16
6 1 11 4.35 33.40
6 1 12 7.19 31.40
6 2 0 511.99 22.16
6 2 1 193.24 8.10
6 2 2 376.74 15.25
6 2 3 443.98 46.80
6 2 4 0.04 8.53
6 2 5 12.85 8.62
6 2 6 59.69 22.59
6 2 7 0.00 10.50
6 2 8 15.22 10.70
6 2 9 1.19 18.05
6 2 10 1.11 48.34
6 2 11 0.28 13.20
6 3 0 791.13 52.19
6 3 1 759.79 21.11
6 3 2 75.71 13.49
6 3 3 52.86 8.97
6 3 4 139.97 14.04
6 3 5 8.27 9.70
6 3 6 0.03 11.80
6 3 7 4.29 24.00
6 3 8 54.18 37.60
6 3 9 1.35 13.30
6 3 10 18.57 14.30
6 3 11 5.57 14.50
6 3 12 145.99 19.10
6 4 0 198.66 19.03
6 4 1 129.10 38.34
6 4 2 318.72 38.79
6 4 3 50.55 9.95
6 4 4 59.33 10.22
6 4 5 10.47 11.40
6 4 6 0.59 12.30
6 4 7 2.12 13.00
6 4 8 9.42 13.70
6 4 9 3.04 14.40
6 4 10 17.62 15.20
6 4 11 4.83 15.00
6 4 12 4.71 13.20
6 5 0 702.62 21.63
6 5 1 382.06 13.94
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6 5 3 0.01 11.30
6 5 4 62.02 16.70
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6 5 6 0.00 13.30
6 5 7 0.98 14.00
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6 6 5 0.15 13.40
6 6 6 5.68 14.20
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6 6 8 1.01 15.00
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6 6 10 17.95 15.50
6 7 0 0.22 7.64
6 7 1 194.88 14.32
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6 7 3 202.53 20.40
6 7 4 20.38 13.90
6 7 5 4.22 14.00
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6 7 7 0.22 14.90
6 7 8 0.00 14.80
6 7 9 8.76 15.30
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6 8 3 142.34 21.10
6 8 4 0.36 14.20
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6 8 6 9.20 14.80
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6 8 8 32.15 15.10
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6 9 4 11.75 15.20
6 9 5 2.40 14.60
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6 10 0 48.34 15.34
6 10 1 0.05 10.32
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6 12 0 9.01 10.90
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7 -13 1 0.73 15.60
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7 -13 4 73.23 14.60
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7 -12 0 283.34 24.70
7 -12 1 209.53 23.70
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7 -12 3 169.22 23.10
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7 -12 5 10.17 13.00
7 -12 11 58.25 31.60
7 -12 12 41.73 32.50
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7 -11 0 216.90 22.20
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7 -11 3 0.85 11.80
7 -11 4 0.90 18.70
7 -11 5 72.48 19.50
7 -11 11 26.66 31.20
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7 -10 0 59.83 17.90
7 -10 1 11.90 10.50
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7 -10 11 0.73 30.30
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7 -10 13 0.02 33.00
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7 -7 12 12.61 11.66
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7 -6 10 12.72 11.25
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7 -5 12 0.03 32.30
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7 -4 11 1.15 31.90
7 -4 12 28.02 34.10
7 -4 13 98.46 42.00
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7 -3 1 1099.20 33.60
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7 -3 7 1.04 19.25
7 -3 8 0.09 24.90
7 -3 9 6.30 27.30
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7 -3 11 4.12 32.30
7 -3 12 3.99 31.90
7 -3 13 3.50 31.50
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7 -2 1 22.33 15.95
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7 -2 4 199.94 14.83
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7 -2 13 17.12 33.30
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7 -1 0 602.92 23.80
7 -1 1 1090.17 20.29
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7 -1 4 46.95 8.52
7 -1 5 2.78 8.54
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7 -1 7 32.18 18.60
7 -1 8 8.89 9.37
7 -1 9 5.45 9.82
7 -1 10 2.28 31.10
7 -1 11 12.84 30.20
7 -1 12 55.20 44.30
7 -1 13 84.01 34.10
7 0 0 580.61 24.15
7 0 1 362.88 19.50
7 0 2 45.50 9.35
7 0 3 26.56 20.60
7 0 4 14.35 6.45
7 0 5 9.10 14.60
7 0 6 22.83 8.46
7 0 7 46.60 21.95
7 0 8 0.06 12.52
7 0 9 5.28 23.96
7 0 10 7.60 20.15
7 0 11 33.55 34.00
7 0 12 0.99 32.40
7 1 0 107.24 11.81
7 1 1 262.22 22.28
7 1 2 110.28 12.95
7 1 3 286.97 14.74
7 1 4 6.29 8.51
7 1 5 8.70 9.29
7 1 6 0.57 9.39
7 1 7 6.07 14.90
7 1 8 2.44 10.59
7 1 9 4.63 10.68
7 1 10 14.75 8.03
7 1 11 37.86 32.30
7 2 0 123.73 6.47
7 2 1 663.32 37.90
7 2 2 145.88 27.95
7 2 3 132.36 14.33
7 2 4 3.23 9.40
7 2 5 35.28 10.25
7 2 6 10.03 10.59
7 2 7 0.57 11.48
7 2 8 88.33 12.79
7 2 9 58.06 19.85
7 2 10 131.38 16.50
7 2 11 45.04 40.89
7 3 0 17.40 6.10
7 3 1 59.12 12.71
7 3 2 54.42 31.69
7 3 3 6.45 9.87
7 3 4 26.13 11.50
7 3 5 14.46 10.92
7 3 6 7.72 11.60
7 3 7 7.46 21.25
7 3 8 66.57 19.00
7 3 9 4.04 13.90
7 3 10 45.66 16.90
7 3 11 6.84 13.95
7 4 0 133.63 13.90
7 4 1 0.63 10.20
7 4 2 121.73 17.50
7 4 3 0.05 11.10
7 4 4 5.62 12.00
7 4 5 6.81 12.80
7 4 6 0.26 13.60
7 4 7 5.52 14.80
7 4 8 2.39 15.20
7 4 9 90.41 18.80
7 4 10 18.26 14.10
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7 5 1 14.21 7.39
7 5 2 72.61 17.80
7 5 3 53.68 12.70
7 5 4 2.10 12.80
7 5 5 1.79 13.60
7 5 6 9.92 14.80
7 5 7 4.66 15.40
7 5 8 0.00 15.70
7 5 9 47.06 15.50
7 5 10 23.85 14.30
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7 6 2 1.72 12.30
7 6 3 21.35 13.20
7 6 4 14.25 14.00
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7 6 7 1.08 15.70
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7 6 9 5.86 14.80
7 7 0 56.63 13.28
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7 7 3 42.24 14.60
7 7 4 11.30 14.30
7 7 5 3.63 15.10
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7 7 7 1.08 15.60
7 7 8 11.46 15.00
7 8 0 13.96 9.33
7 8 1 41.23 10.06
7 8 2 0.07 14.40
7 8 3 10.05 15.00
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7 9 5 9.85 15.00
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7 10 0 119.21 15.91
7 10 1 78.70 16.70
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8 -16 1 11.20 17.30
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8 -16 4 190.46 25.80
8 -16 5 152.10 23.90
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8 -15 1 406.31 33.70
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8 -14 0 167.76 28.90
8 -14 1 68.64 18.70
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8 -14 4 270.02 27.80
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8 -13 11 17.70 31.50
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8 -12 11 15.21 33.00
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8 -11 1 26.99 13.10
8 -11 2 196.12 22.10
8 -11 3 626.78 31.80
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8 -3 5 1.32 9.58
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8 -3 8 0.02 28.60
8 -3 9 0.98 30.80
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8 -2 1 800.76 30.30
8 -2 2 394.95 18.80
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8 -2 4 28.97 9.10
8 -2 5 1.85 9.23
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8 -2 8 0.25 14.60
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8 -1 1 11.10 15.10
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8 0 7 0.32 10.44
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8 0 11 0.02 32.70
8 1 0 62.71 9.70
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8 1 3 229.41 10.44
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8 1 5 0.19 9.08
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8 1 7 19.38 11.41
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8 1 10 51.91 36.49
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8 2 5 25.81 9.27
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8 2 8 49.81 17.08
8 2 9 5.54 13.50
8 2 10 39.11 13.80
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8 3 2 222.09 20.30
8 3 3 40.88 17.70
8 3 4 52.70 24.00
8 3 5 1.26 11.52
8 3 6 4.46 13.30
8 3 7 1.80 9.72
8 3 8 8.34 9.82
8 3 9 47.38 23.95
8 3 10 18.14 14.10
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8 5 5 135.68 20.50
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9 -14 1 125.91 28.70
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9 -13 0 194.89 27.80
9 -13 1 546.74 33.10
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9 -12 0 0.89 16.30
9 -12 1 51.88 16.30
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9 -12 9 0.06 32.30
9 -12 10 0.02 32.80
9 -11 0 309.18 25.50
9 -11 1 487.80 27.70
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9 -11 3 200.63 24.20
9 -11 4 72.25 15.10
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9 -11 9 0.21 32.60
9 -11 10 15.96 35.10
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9 -10 1 300.78 27.10
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9 -10 3 0.36 14.40
9 -10 4 134.33 21.90
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9 -9 0 0.81 12.80
9 -9 1 14.63 13.20
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9 -9 3 186.87 23.30
9 -9 4 376.96 25.90
9 -9 5 32.16 14.50
9 -9 8 0.12 30.80
9 -9 9 0.54 33.50
9 -9 10 0.15 34.70
9 -9 11 2.34 34.70
9 -9 12 11.32 31.30
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9 -8 2 116.00 19.70
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9 -8 9 7.55 33.70
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9 -7 3 0.11 13.10
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9 -6 1 226.12 22.50
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9 -5 5 9.95 14.90
9 -5 6 0.18 11.48
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9 -5 8 8.80 32.20
9 -5 9 9.82 33.60
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9 -4 0 0.40 11.90
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9 -4 4 4.58 10.56
9 -4 5 3.55 10.68
9 -4 6 24.68 10.99
9 -4 7 3.99 14.20
9 -4 8 4.58 32.20
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9 -4 11 2.34 34.50
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9 -3 3 10.85 9.97
9 -3 4 13.40 10.38
9 -3 5 18.87 10.54
9 -3 6 0.25 12.45
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9 -3 8 0.81 32.10
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9 -1 9 23.01 32.60
9 -1 10 2.04 32.60
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9 0 9 0.74 11.80
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9 1 6 2.25 13.45
9 1 7 3.13 12.25
9 1 8 56.02 15.60
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9 2 1 0.11 11.90
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9 2 5 27.20 12.86
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9 3 1 1.20 12.50
9 3 2 126.35 22.35
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10 -12 1 13.94 17.50
10 -12 2 185.06 29.10
10 -12 3 316.34 26.20
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10 -12 5 54.26 16.30
10 -12 8 0.01 33.20
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10 -11 3 8.16 16.20
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10 -10 4 12.04 16.60
10 -10 5 20.24 16.10
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10 -9 1 29.24 15.50
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10 -9 4 5.61 15.80
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10 -6 5 16.84 12.29
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10 -5 4 2.01 12.29
10 -5 5 0.98 12.26
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10 -4 5 0.05 13.00
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10 -3 3 5.19 17.95
10 -3 4 6.34 11.38
10 -3 5 0.00 11.30
10 -3 6 8.00 11.55
10 -3 7 10.68 33.20
10 -3 8 18.06 33.80
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10 -2 1 16.92 12.40
10 -2 2 1.92 11.51
10 -2 3 181.72 18.03
10 -2 4 32.77 11.75
10 -2 5 18.48 11.79
10 -2 6 45.73 16.08
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10 -2 8 26.41 11.44
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10 -1 1 228.66 21.00
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10 -1 4 98.71 29.80
10 -1 5 1.10 30.00
10 -1 6 0.00 23.90
10 -1 7 0.09 14.45
10 -1 8 12.72 11.72
10 -1 9 0.06 31.50
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10 0 3 19.02 13.40
10 0 4 3.24 12.75
10 0 5 1.91 12.60
10 0 6 37.39 15.50
10 0 7 32.27 18.99
10 0 8 10.40 22.05
10 0 9 2.61 13.80
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10 1 1 90.32 13.50
10 1 2 188.44 21.40
10 1 3 26.03 14.30
10 1 4 84.51 13.39
10 1 5 20.67 13.45
10 1 6 2.93 12.96
10 1 7 0.02 13.90
10 1 8 2.97 13.60
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10 2 1 67.33 18.90
10 2 2 354.38 25.30
10 2 3 6.51 14.60
10 2 4 32.15 15.50
10 2 5 0.51 14.70
10 2 6 0.22 14.80
10 2 7 0.00 14.20
10 2 8 0.27 13.80
10 3 0 13.44 14.00
10 3 1 0.27 14.40
10 3 2 15.94 15.40
10 3 3 49.98 21.50
10 3 4 3.01 15.80
10 3 5 29.53 16.10
10 3 6 10.15 15.10
10 3 7 15.74 14.90
10 4 0 19.43 15.10
10 4 1 102.79 22.50
10 4 2 0.59 15.90
10 4 3 73.00 16.60
10 4 4 1.16 16.10
10 4 5 12.55 16.00
10 4 6 11.57 15.40
10 5 0 133.21 22.20
10 5 1 121.85 23.60
10 5 2 0.41 16.30
10 5 3 0.00 16.20
10 5 4 4.11 15.90
10 5 5 1.01 15.70
10 6 0 21.20 16.60
10 6 1 10.34 16.20
10 6 2 26.15 16.60
10 6 3 45.80 16.50
10 6 4 44.71 21.50
10 7 0 14.28 16.60
10 7 1 94.63 23.10
10 7 2 128.63 21.90
10 7 3 100.39 22.60
10 8 0 9.56 16.20
10 8 1 11.00 16.10
10 8 2 12.73 15.60
10 9 0 38.71 16.00
11 -14 0 15.47 19.90
11 -14 1 9.51 19.30
11 -14 2 3.37 18.90
11 -14 3 25.44 18.50
11 -13 0 0.60 18.90
11 -13 1 29.78 18.90
11 -13 2 173.63 27.40
11 -13 3 125.29 25.90
11 -13 4 17.94 17.30
11 -12 0 14.14 18.20
11 -12 1 70.80 27.40
11 -12 2 88.44 26.20
11 -12 3 31.87 17.80
11 -12 4 9.65 16.90
11 -11 0 0.11 17.00
11 -11 1 17.22 17.40
11 -11 2 21.48 17.80
11 -11 3 3.45 17.10
11 -11 4 74.61 16.90
11 -11 5 49.60 23.50
11 -11 6 34.33 34.40
11 -11 7 20.47 35.10
11 -10 0 45.70 17.50
11 -10 1 14.57 17.40
11 -10 2 32.86 18.00
11 -10 3 53.51 17.60
11 -10 4 102.54 16.80
11 -10 5 45.59 41.19
11 -10 6 2.90 34.20
11 -10 7 0.27 35.40
11 -10 8 1.50 34.80
11 -9 0 44.96 25.70
11 -9 1 13.72 17.20
11 -9 2 0.03 17.00
11 -9 3 1.83 17.00
11 -9 4 23.74 17.20
11 -9 5 38.74 15.28
11 -9 6 27.49 34.90
11 -9 7 36.52 35.50
11 -9 8 22.33 35.30
11 -8 0 0.61 14.50
11 -8 1 36.54 15.60
11 -8 2 29.02 15.90
11 -8 3 22.27 15.90
11 -8 4 20.04 13.91
11 -8 5 33.21 29.40
11 -8 6 3.58 34.90
11 -8 7 0.34 34.40
11 -8 8 8.84 34.70
11 -8 9 21.00 34.80
11 -7 0 34.65 15.00
11 -7 1 20.93 15.90
11 -7 2 1.42 15.60
11 -7 3 0.25 13.69
11 -7 4 0.06 14.03
11 -7 5 5.64 14.00
11 -7 6 0.32 14.32
11 -7 7 3.08 34.20
11 -7 8 19.55 35.30
11 -7 9 31.36 30.70
11 -6 0 0.91 14.70
11 -6 1 1.63 14.50
11 -6 2 15.14 13.01
11 -6 3 2.07 13.23
11 -6 4 31.46 13.45
11 -6 5 18.87 13.45
11 -6 6 61.82 13.36
11 -6 7 39.72 34.10
11 -6 8 0.07 33.50
11 -6 9 0.17 30.80
11 -5 0 0.28 13.50
11 -5 1 13.43 14.20
11 -5 2 320.93 56.24
11 -5 3 274.47 20.29
11 -5 4 151.76 19.66
11 -5 5 57.26 12.98
11 -5 6 17.71 17.90
11 -5 7 8.09 33.00
11 -5 8 0.23 33.50
11 -5 9 29.46 30.10
11 -4 0 60.93 14.20
11 -4 1 71.64 21.80
11 -4 2 202.72 25.00
11 -4 3 3.73 23.90
11 -4 4 0.77 13.06
11 -4 5 1.21 20.70
11 -4 6 12.54 12.55
11 -4 7 42.74 13.10
11 -4 8 50.40 33.40
11 -4 9 57.76 37.60
11 -3 0 0.24 14.30
11 -3 1 43.79 14.70
11 -3 2 5.28 14.20
11 -3 3 11.60 14.20
11 -3 4 80.57 38.10
11 -3 5 56.64 21.89
11 -3 6 57.35 33.40
11 -3 7 93.33 24.50
11 -3 8 16.57 31.00
11 -2 0 5.55 13.60
11 -2 1 245.52 22.10
11 -2 2 61.66 14.30
11 -2 3 150.36 21.20
11 -2 4 60.80 25.50
11 -2 5 21.48 32.30
11 -2 6 15.26 20.40
11 -2 7 26.82 16.20
11 -2 8 4.72 30.40
11 -1 0 33.95 13.10
11 -1 1 188.69 21.80
11 -1 2 92.83 20.10
11 -1 3 49.86 14.80
11 -1 4 2.43 14.20
11 -1 5 15.61 29.09
11 -1 6 42.47 20.99
11 -1 7 30.55 14.15
11 -1 8 13.36 12.20
11 0 0 0.06 13.90
11 0 1 0.92 14.50
11 0 2 67.87 15.40
11 0 3 10.97 15.50
11 0 4 204.16 22.40
11 0 5 66.01 19.50
11 0 6 25.72 14.30
11 0 7 14.15 13.20
11 1 0 42.04 15.30
11 1 1 34.27 15.50
11 1 2 160.39 22.80
11 1 3 6.70 15.80
11 1 4 34.61 16.10
11 1 5 15.17 15.50
11 1 6 2.11 14.80
11 1 7 3.89 13.80
11 2 0 194.74 22.70
11 2 1 1.95 15.40
11 2 2 0.09 15.60
11 2 3 131.64 22.00
11 2 4 19.51 15.90
11 2 5 34.44 15.70
11 2 6 14.31 15.10
11 3 0 0.27 15.50
11 3 1 44.87 16.30
11 3 2 86.10 22.80
11 3 3 204.36 24.30
11 3 4 48.14 16.50
11 3 5 18.43 15.50
11 4 0 72.46 16.50
11 4 1 157.16 24.00
11 4 2 35.25 16.70
11 4 3 23.14 16.40
11 4 4 0.76 15.60
11 5 0 6.58 16.30
11 5 1 8.17 16.40
11 5 2 14.71 16.60
11 5 3 6.16 15.80
11 6 0 37.22 16.80
11 6 1 127.53 23.50
11 6 2 149.76 23.20
11 7 0 72.92 16.40
11 7 1 85.56 22.40
11 8 0 8.00 15.30
12 -13 0 0.18 18.60
12 -13 1 5.65 18.10
12 -13 2 28.75 18.10
12 -12 0 2.78 18.20
12 -12 1 33.75 18.60
12 -12 2 1.01 17.50
12 -12 3 87.19 23.60
12 -12 4 138.76 23.60
12 -11 0 9.61 17.70
12 -11 1 13.81 17.70
12 -11 2 71.45 18.00
12 -11 3 202.37 23.50
12 -11 4 102.72 19.61
12 -11 5 33.19 34.80
12 -10 0 1.20 17.90
12 -10 1 1.69 18.00
12 -10 2 5.59 17.60
12 -10 3 0.90 14.98
12 -10 4 23.16 14.78
12 -10 5 47.23 35.00
12 -10 6 11.16 34.80
12 -9 0 0.96 17.60
12 -9 1 29.65 18.60
12 -9 2 42.45 18.20
12 -9 3 7.41 16.60
12 -9 4 28.19 15.21
12 -9 5 119.12 23.25
12 -9 6 58.26 34.20
12 -8 0 22.82 16.10
12 -8 1 79.54 24.60
12 -8 2 66.92 17.00
12 -8 3 91.77 18.55
12 -8 4 45.71 18.49
12 -8 5 34.22 13.81
12 -8 6 1.96 33.00
12 -8 7 21.91 34.00
12 -7 0 19.63 16.10
12 -7 1 56.26 16.50
12 -7 2 1.03 16.10
12 -7 3 0.84 14.61
12 -7 4 35.58 14.16
12 -7 5 63.50 13.63
12 -7 6 115.19 40.30
12 -7 7 88.98 39.80
12 -6 0 23.03 16.70
12 -6 1 11.89 16.30
12 -6 2 151.95 25.30
12 -6 3 103.25 16.70
12 -6 4 87.76 41.30
12 -6 5 34.41 18.14
12 -6 6 38.52 16.10
12 -6 7 29.85 30.50
12 -5 0 53.41 23.00
12 -5 1 111.02 23.40
12 -5 2 204.49 24.10
12 -5 3 2.60 14.90
12 -5 4 12.92 14.30
12 -5 5 3.91 22.55
12 -5 6 16.84 17.55
12 -5 7 55.99 38.10
12 -4 0 12.78 14.40
12 -4 1 0.64 15.10
12 -4 2 13.63 15.40
12 -4 3 5.46 15.30
12 -4 4 15.27 14.60
12 -4 5 117.81 19.10
12 -4 6 141.04 39.40
12 -4 7 61.75 36.50
12 -3 0 22.06 15.60
12 -3 1 100.60 23.40
12 -3 2 59.84 15.80
12 -3 3 144.83 22.00
12 -3 4 88.57 20.90
12 -3 5 50.73 14.50
12 -3 6 1.96 13.20
12 -2 0 43.40 15.80
12 -2 1 5.12 15.00
12 -2 2 2.14 15.10
12 -2 3 71.05 15.50
12 -2 4 1.78 14.30
12 -2 5 2.19 13.80
12 -2 6 0.02 13.30
12 -1 0 0.06 14.70
12 -1 1 16.57 14.70
12 -1 2 158.43 21.40
12 -1 3 19.54 14.80
12 -1 4 30.79 14.70
12 -1 5 16.91 13.90
12 -1 6 1.07 13.40
12 0 0 10.92 14.70
12 0 1 34.26 14.90
12 0 2 189.74 23.20
12 0 3 0.15 15.00
12 0 4 0.32 14.30
12 0 5 0.38 13.70
12 1 0 51.25 15.70
12 1 1 17.87 16.10
12 1 2 33.25 15.80
12 1 3 0.18 15.50
12 1 4 3.17 15.00
12 1 5 4.73 14.20
12 2 0 5.27 16.10
12 2 1 29.33 16.90
12 2 2 3.30 16.20
12 2 3 29.87 16.50
12 2 4 8.67 15.30
12 3 0 149.63 23.50
12 3 1 141.06 25.10
12 3 2 28.51 17.00
12 3 3 4.54 16.20
12 4 0 15.92 17.10
12 4 1 20.51 16.80
12 4 2 0.05 16.30
12 5 0 23.25 16.70
12 5 1 20.49 16.30
12 6 0 69.31 22.40
13 -11 0 8.23 17.10
13 -11 1 18.48 16.80
13 -11 2 41.25 16.10
13 -10 0 0.21 18.00
13 -10 1 0.17 17.30
13 -10 2 14.32 17.30
13 -10 3 63.53 20.90
13 -9 0 79.93 18.70
13 -9 1 166.49 26.10
13 -9 2 86.91 17.60
13 -9 3 135.90 23.40
13 -9 4 73.85 20.40
13 -8 0 46.93 17.70
13 -8 1 55.99 23.20
13 -8 2 9.67 16.40
13 -8 3 4.24 15.60
13 -8 4 3.04 15.10
13 -7 0 1.22 16.10
13 -7 1 0.03 16.20
13 -7 2 80.02 16.40
13 -7 3 76.40 21.40
13 -7 4 102.77 20.60
13 -6 0 3.22 16.20
13 -6 1 27.85 16.80
13 -6 2 195.57 22.90
13 -6 3 76.07 21.90
13 -6 4 16.09 15.10
13 -6 5 4.24 13.60
13 -5 0 8.18 16.00
13 -5 1 0.29 15.80
13 -5 2 9.80 15.90
13 -5 3 0.77 15.40
13 -5 4 0.00 14.60
13 -5 5 1.54 13.90
13 -4 0 39.98 15.30
13 -4 1 142.97 22.40
13 -4 2 117.06 22.30
13 -4 3 161.83 22.00
13 -4 4 32.53 14.40
13 -4 5 3.40 13.10
13 -3 0 104.26 22.20
13 -3 1 104.37 22.10
13 -3 2 2.31 15.10
13 -3 3 15.53 14.80
13 -3 4 0.25 13.70
13 -2 0 0.38 15.70
13 -2 1 1.25 15.60
13 -2 2 72.53 22.50
13 -2 3 1.86 14.80
13 -2 4 2.06 14.30
13 -1 0 192.34 24.70
13 -1 1 112.99 22.40
13 -1 2 84.96 22.10
13 -1 3 18.29 15.00
13 -1 4 8.81 14.50
13 0 0 81.65 16.30
13 0 1 10.68 15.70
13 0 2 7.55 15.10
13 0 3 2.97 14.60
13 1 0 7.56 15.40
13 1 1 25.56 15.20
13 1 2 58.85 20.30
13 2 0 83.75 21.80
13 2 1 39.09 15.20
13 2 2 1.49 14.60
13 3 0 17.66 15.80
13 3 1 0.04 15.10
13 4 0 23.75 15.60
14 -9 0 13.82 16.60
14 -8 0 0.57 17.10
14 -8 1 0.15 16.60
14 -7 0 85.06 21.90
14 -7 1 160.88 22.20
14 -7 2 216.82 22.20
14 -6 0 59.68 16.20
14 -6 1 33.89 15.60
14 -6 2 2.99 14.40
14 -5 0 44.83 16.80
14 -5 1 35.35 16.50
14 -5 2 2.56 15.40
14 -4 0 28.35 16.20
14 -4 1 11.55 15.30
14 -4 2 8.47 14.80
14 -3 0 0.79 14.80
14 -3 1 3.38 14.70
14 -3 2 3.36 14.20
14 -2 0 48.36 15.40
14 -2 1 67.52 14.90
14 -1 0 9.71 15.50
14 -1 1 0.41 15.00
14 0 0 1.04 15.60
14 1 0 0.98 15.10
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 32706
_olex2_submission_original_sample_id n3560
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_THETM01_X1
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Despite long exposure times, the crystal did not exhibit observable intensity to a resolution higher than 1.1 angstrom.
;
_vrf_PLAT431_X1
;
PROBLEM: Short Inter HL..A Contact F4 .. O4 .. 2.48 Ang.
RESPONSE: The contact is probably owing to the disordered triflate that is not always in that position.
;
# end Validation Reply Form