# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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data_TMPF-88
_database_code_depnum_ccdc_archive 'CCDC 1429138'
_audit_update_record
;
2015-11-29 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_TMPF-88
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 479 Ang3
RESPONSE: The structure corresponds to a porous metal-organic framework
;
# Added during the CSD deposition process: Sunday 29th of November 2015 11:17:07 AM
# end Validation Reply Form
_audit_creation_date 2015-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C38 H23 F12 N6 O9.5 Zn3, 1.2(O)'
_chemical_formula_sum 'C38 H23 F12 N6 O10.70 Zn3'
_chemical_formula_weight 1158.95
_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'
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'
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 36.4551(9)
_cell_length_b 18.1156(4)
_cell_length_c 14.1588(4)
_cell_angle_alpha 90
_cell_angle_beta 93.8165(13)
_cell_angle_gamma 90
_cell_volume 9329.8(4)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9990
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 65.09
_cell_measurement_theta_min 2.43
_shelx_estimated_absorpt_T_max 0.946
_shelx_estimated_absorpt_T_min 0.605
_exptl_absorpt_coefficient_mu 2.793
_exptl_absorpt_correction_T_max 0.7526
_exptl_absorpt_correction_T_min 0.5015
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.6664.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.650
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 4613
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0598
_diffrn_reflns_av_unetI/netI 0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max 42
_diffrn_reflns_limit_h_min -41
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 38120
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full 65.299
_diffrn_reflns_theta_max 65.299
_diffrn_reflns_theta_min 2.429
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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 6378
_reflns_number_total 7787
_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 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'Bruker APEX-II CCD'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.656
_refine_diff_density_min -0.689
_refine_diff_density_rms 0.138
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 650
_refine_ls_number_reflns 7787
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0517
_refine_ls_R_factor_gt 0.0406
_refine_ls_restrained_S_all 1.064
_refine_ls_shift/su_max 0.010
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1283
_refine_ls_wR_factor_ref 0.1593
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2. Others
Fixed Sof: Zn3(0.5) O1(0.5) H1A(0.5) H1B(0.5) Zn3A(0.5) O3(0.5)
Fixed Uiso: H2AA(0.039) H25(0.033) H1AA(0.032) H33(0.036) H35(0.041)
H39(0.038) H42(0.036) H50(0.041) H58(0.037) H59(0.058) H62(0.053) H63(0.061)
H64(0.04) H13A(0.054) H13B(0.054) H5(0.033) H1A(0.121) H1B(0.121)
Fixed X: H2AA(0.291101) H25(0.334) H1AA(0.2958) H33(0.287499) H35(0.4159)
H39(0.604) H42(0.4011) H50(0.465301) H58(0.391201) H59(0.5997) H62(0.4801)
H63(0.4295) H64(0.5495) H13A(0.2672) H13B(0.3) H5(0.2676) H1A(0.395201)
H1B(0.406699)
Fixed Y: H2AA(0.5676) H25(0.511101) H1AA(0.9151) H33(0.8146) H35(0.209399)
H39(0.257) H42(0.9286) H50(0.145201) H58(0.8337) H59(0.3247) H62(0.3069)
H63(0.367801) H64(0.1925) H13A(0.323001) H13B(0.327101) H5(1.0806)
H1A(0.608201) H1B(0.6499)
Fixed Z: H2AA(0.383801) H25(0.151201) H1AA(0.600801) H33(0.5017)
H35(0.206599) H39(-0.1595) H42(0.5362) H50(0.1534) H58(0.4275) H59(0.1091)
H62(-0.0342) H63(0.0166) H64(-0.148499) H13A(0.076099) H13B(0.030399)
H5(0.8455) H1A(0.3167) H1B(0.2276)
3.a Aromatic/amide H refined with riding coordinates:
C9(H9), C14(H14), C20(H20), C24(H24), C26(H26), C6(H6)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.20871(2) 0.89220(3) 1.06614(3) 0.02371(15) Uani 1 1 d . . . . .
Zn2 Zn 0.31649(2) 0.34436(3) 0.19901(4) 0.02716(16) Uani 1 1 d . . . . .
Zn3 Zn 0.31873(18) 0.6767(5) 0.2312(7) 0.0212(8) Uani 0.5 1 d . . P A 1
O2 O 0.24320(8) 0.89613(15) 0.9686(2) 0.0324(6) Uani 1 1 d . . . . .
F7 F 0.50938(7) 0.09370(15) -0.1330(2) 0.0465(6) Uani 1 1 d . . . . .
N13 N 0.31415(9) 0.56897(17) 0.2587(2) 0.0289(7) Uani 1 1 d . . . . .
C2AA C 0.29964(12) 0.5397(2) 0.3348(3) 0.0323(9) Uani 1 1 d . . . . .
H2AA H 0.2911 0.5676 0.3838 0.039 Uiso 1 1 d . . . . .
N21 N 0.31415(8) 0.44752(16) 0.2500(2) 0.0253(6) Uani 1 1 d . . . . .
N23 N 0.20114(9) 0.96744(17) 1.1670(2) 0.0282(7) Uani 1 1 d . . . . .
F0AA F 0.55042(8) 0.07570(17) 0.0281(2) 0.0568(8) Uani 1 1 d . . . . .
C25 C 0.32297(11) 0.5091(2) 0.2085(3) 0.0276(8) Uani 1 1 d . . . . .
H25 H 0.3340 0.5111 0.1512 0.033 Uiso 1 1 d . . . . .
C1AA C 0.31548(10) 0.8972(2) 0.5689(3) 0.0269(8) Uani 1 1 d . . . . .
H1AA H 0.2958 0.9151 0.6008 0.032 Uiso 1 1 d . . . . .
C33 C 0.31022(11) 0.8380(2) 0.5081(3) 0.0301(8) Uani 1 1 d . . . . .
H33 H 0.2875 0.8146 0.5017 0.036 Uiso 1 1 d . . . . .
C35 C 0.42830(11) 0.2281(2) 0.1566(3) 0.0338(9) Uani 1 1 d . . . . .
H35 H 0.4159 0.2094 0.2066 0.041 Uiso 1 1 d . . . . .
C36 C 0.64517(11) 0.3297(2) -0.0292(3) 0.0304(8) Uani 1 1 d . . . . .
C38 C 0.35011(10) 0.9307(2) 0.5833(3) 0.0243(7) Uani 1 1 d . . . . .
C39 C 0.59229(11) 0.2575(2) -0.1030(3) 0.0319(8) Uani 1 1 d . . . . .
H39 H 0.6040 0.2570 -0.1595 0.038 Uiso 1 1 d . . . . .
C40 C 0.47736(10) 0.2177(2) 0.0512(3) 0.0307(8) Uani 1 1 d . . . . .
C41 C 0.60779(10) 0.2957(2) -0.0270(3) 0.0336(9) Uani 1 1 d . . . . .
C42 C 0.37818(10) 0.9060(2) 0.5292(3) 0.0305(8) Uani 1 1 d . . . . .
H42 H 0.4011 0.9286 0.5362 0.036 Uiso 1 1 d . . . . .
C45 C 0.33891(10) 0.8128(2) 0.4562(2) 0.0252(7) Uani 1 1 d . . . . .
C46 C 0.38189(12) 0.3292(3) 0.1413(3) 0.0409(10) Uani 1 1 d . . . . .
O75 O 0.37206(11) 0.3902(2) 0.1080(3) 0.0653(12) Uani 1 1 d . . . . .
C49 C 0.54118(10) 0.2218(2) -0.0137(3) 0.0307(8) Uani 1 1 d . . . . .
C50 C 0.45812(11) 0.1898(2) 0.1250(3) 0.0339(9) Uani 1 1 d . . . . .
H50 H 0.4653 0.1452 0.1534 0.041 Uiso 1 1 d . . . . .
C56 C 0.50727(10) 0.1736(2) 0.0031(3) 0.0305(8) Uani 1 1 d . . . . .
C58 C 0.37245(11) 0.8483(2) 0.4648(3) 0.0313(8) Uani 1 1 d . . . . .
H58 H 0.3912 0.8337 0.4275 0.037 Uiso 1 1 d . . . . .
C59 C 0.58943(13) 0.2988(3) 0.0571(3) 0.0480(12) Uani 1 1 d . . . . .
H59 H 0.5997 0.3247 0.1091 0.058 Uiso 1 1 d . . . . .
C61 C 0.41678(11) 0.2936(2) 0.1149(3) 0.0364(9) Uani 1 1 d . . . . .
C62 C 0.46668(13) 0.2860(2) 0.0128(4) 0.0445(11) Uani 1 1 d . . . . .
H62 H 0.4801 0.3069 -0.0342 0.053 Uiso 1 1 d . . . . .
C63 C 0.43655(15) 0.3229(3) 0.0437(4) 0.0510(13) Uani 1 1 d . . . . .
H63 H 0.4295 0.3678 0.0166 0.061 Uiso 1 1 d . . . . .
C64 C 0.55938(11) 0.2195(2) -0.0968(3) 0.0330(9) Uani 1 1 d . . . . .
H64 H 0.5495 0.1925 -0.1485 0.040 Uiso 1 1 d . . . . .
O5 O 0.36189(8) 0.29197(17) 0.1944(2) 0.0428(7) Uani 1 1 d . . . . .
N7 N 0.27800(9) 0.28921(17) 0.2685(2) 0.0282(7) Uani 1 1 d . . . . .
O11 O 0.65768(8) 0.3621(2) 0.0442(2) 0.0509(9) Uani 1 1 d . . . . .
O12 O 0.33698(8) 0.67702(18) 0.0997(2) 0.0408(7) Uani 1 1 d . . . . .
O13 O 0.28747(8) 0.34698(16) 0.0732(2) 0.0358(6) Uani 1 1 d . . . . .
H13A H 0.2672 0.3230 0.0761 0.054 Uiso 1 1 d . . . . .
H13B H 0.3000 0.3271 0.0304 0.054 Uiso 1 1 d . . . . .
N14 N 0.27360(9) 0.72915(17) 0.2066(2) 0.0284(7) Uani 1 1 d . . . . .
F2AA F 0.40265(7) 0.92877(16) 0.7397(2) 0.0480(7) Uani 1 1 d . . . . .
F1AA F 0.31564(7) 1.07555(14) 0.56332(18) 0.0418(6) Uani 1 1 d . . . . .
F6 F 0.49631(8) 0.05488(14) 0.0722(2) 0.0513(7) Uani 1 1 d . . . . .
F3AA F 0.42063(7) 1.01525(18) 0.6511(2) 0.0538(7) Uani 1 1 d . . . . .
C9 C 0.32315(10) 0.9220(2) 0.7761(3) 0.0273(8) Uani 1 1 d . . . . .
H9 H 0.3375 0.8822 0.7598 0.033 Uiso 1 1 calc R . . . .
O10 O 0.30900(9) 0.70085(15) 0.40814(19) 0.0381(7) Uani 1 1 d . . . . .
C11 C 0.27628(10) 0.9720(2) 0.8691(2) 0.0241(7) Uani 1 1 d . . . . .
C14 C 0.29796(11) 0.9128(2) 0.8433(3) 0.0279(8) Uani 1 1 d . . . . .
H14 H 0.2954 0.8670 0.8717 0.034 Uiso 1 1 calc R . . . .
C15 C 0.52128(12) 0.1079(2) 0.0636(3) 0.0387(10) Uani 1 1 d . . . . .
F16 F 0.37089(8) 1.06831(15) 0.5225(2) 0.0529(7) Uani 1 1 d . . . . .
F17 F 0.53219(8) 0.12888(17) 0.1516(2) 0.0523(7) Uani 1 1 d . . . . .
O19 O 0.23177(8) 1.01546(17) 0.9720(2) 0.0390(7) Uani 1 1 d . . . . .
C20 C 0.25264(11) 0.2430(2) 0.2332(3) 0.0305(8) Uani 1 1 d . . . . .
H20 H 0.2529 0.2223 0.1731 0.037 Uiso 1 1 calc R . . . .
C21 C 0.35539(10) 0.9950(2) 0.6548(3) 0.0248(7) Uani 1 1 d . . . . .
N22 N 0.23248(9) 0.80841(17) 1.1425(2) 0.0299(7) Uani 1 1 d . . . . .
C23 C 0.39422(11) 0.9951(3) 0.7066(3) 0.0378(10) Uani 1 1 d . . . . .
C24 C 0.30681(10) 1.0492(2) 0.7605(3) 0.0282(8) Uani 1 1 d . . . . .
H24 H 0.3101 1.0955 0.7339 0.034 Uiso 1 1 calc R . . . .
C0AA C 0.33211(11) 0.7494(2) 0.3894(3) 0.0281(8) Uani 1 1 d . . . . .
C26 C 0.55626(12) 0.2630(3) 0.0622(3) 0.0467(12) Uani 1 1 d . . . . .
H26 H 0.5438 0.2665 0.1172 0.056 Uiso 1 1 calc R . . . .
C27 C 0.35036(12) 1.0672(2) 0.5960(3) 0.0355(9) Uani 1 1 d . . . . .
C28 C 0.24859(10) 0.9621(2) 0.9403(3) 0.0270(8) Uani 1 1 d . . . . .
C29 C 0.32747(9) 0.9901(2) 0.7321(2) 0.0229(7) Uani 1 1 d . . . . .
F1 F 0.48058(7) 0.19666(16) -0.15266(19) 0.0496(7) Uani 1 1 d . . . . .
F2 F 0.35925(8) 1.12750(14) 0.6482(2) 0.0505(7) Uani 1 1 d . . . . .
F3 F 0.45695(7) 0.10866(17) -0.0756(2) 0.0532(7) Uani 1 1 d . . . . .
F4 F 0.39580(7) 1.04140(18) 0.7796(2) 0.0542(8) Uani 1 1 d . . . . .
C5 C 0.28143(10) 1.0403(2) 0.8278(3) 0.0276(8) Uani 1 1 d . . . . .
H5 H 0.2676 1.0806 0.8455 0.033 Uiso 1 1 d . . . . .
C6 C 0.26326(11) 0.7711(2) 0.1313(3) 0.0293(8) Uani 1 1 d . . . . .
H6 H 0.2763 0.7737 0.0770 0.035 Uiso 1 1 calc R . . . .
O0AA O 0.34874(8) 0.74795(15) 0.3142(2) 0.0350(6) Uani 1 1 d . . . . .
C2 C 0.48874(11) 0.1428(3) -0.0901(3) 0.0384(10) Uani 1 1 d . . . . .
O1 O 0.3860(3) 0.6196(5) 0.2502(8) 0.083(3) Uani 0.5 1 d . . P A 2
H1A H 0.3952 0.6082 0.3167 0.121 Uiso 0.5 1 d . . P B 2
H1B H 0.4067 0.6499 0.2276 0.121 Uiso 0.5 1 d . . P C 2
O1AA O 0.5899(5) 0.5283(7) 0.3827(17) 0.263(14) Uani 0.70(2) 1 d . . . . .
Zn3A Zn 0.32721(18) 0.6725(6) 0.2312(7) 0.0266(10) Uani 0.5 1 d . . P A 2
O3 O 0.3861(8) 0.5255(15) 0.417(2) 0.273(15) Uani 0.5 1 d . . P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0272(3) 0.0258(3) 0.0190(3) -0.00252(17) 0.00820(18) -0.00378(18)
Zn2 0.0315(3) 0.0234(3) 0.0282(3) -0.00095(19) 0.0134(2) 0.00560(19)
Zn3 0.026(2) 0.0186(9) 0.0205(8) -0.0009(5) 0.0104(16) 0.0028(16)
O2 0.0340(15) 0.0358(15) 0.0291(15) -0.0002(11) 0.0153(11) -0.0045(11)
F7 0.0406(14) 0.0505(15) 0.0502(16) -0.0226(12) 0.0158(12) -0.0062(11)
N13 0.0421(18) 0.0254(15) 0.0206(16) 0.0012(12) 0.0122(13) 0.0033(13)
C2AA 0.054(2) 0.0232(18) 0.0218(19) -0.0008(14) 0.0155(17) 0.0050(17)
N21 0.0317(16) 0.0244(15) 0.0210(15) -0.0009(12) 0.0105(12) 0.0051(12)
N23 0.0403(18) 0.0248(15) 0.0206(16) -0.0008(12) 0.0098(13) -0.0026(13)
F0AA 0.0425(15) 0.0601(18) 0.070(2) 0.0035(14) 0.0241(14) 0.0232(13)
C25 0.038(2) 0.0242(18) 0.0221(18) -0.0011(14) 0.0098(15) 0.0014(15)
C1AA 0.0237(18) 0.0333(19) 0.0246(19) -0.0057(15) 0.0080(14) -0.0030(14)
C33 0.0263(19) 0.0326(19) 0.032(2) -0.0047(16) 0.0071(15) -0.0103(15)
C35 0.0276(19) 0.039(2) 0.037(2) -0.0037(17) 0.0174(16) -0.0020(17)
C36 0.028(2) 0.035(2) 0.030(2) -0.0057(16) 0.0120(16) -0.0023(16)
C38 0.0280(18) 0.0268(18) 0.0185(18) -0.0020(13) 0.0046(13) -0.0035(14)
C39 0.030(2) 0.040(2) 0.027(2) -0.0057(16) 0.0108(15) -0.0006(16)
C40 0.0194(18) 0.038(2) 0.036(2) -0.0053(16) 0.0076(15) -0.0033(15)
C41 0.0201(18) 0.045(2) 0.037(2) -0.0102(17) 0.0116(15) -0.0043(16)
C42 0.0247(18) 0.041(2) 0.026(2) -0.0077(16) 0.0090(14) -0.0060(16)
C45 0.034(2) 0.0247(17) 0.0169(18) -0.0010(13) 0.0028(14) 0.0009(15)
C46 0.037(2) 0.043(2) 0.044(3) -0.0120(19) 0.0135(19) 0.0038(19)
O75 0.061(2) 0.046(2) 0.094(3) 0.0089(19) 0.043(2) 0.0219(17)
C49 0.0204(18) 0.039(2) 0.034(2) -0.0067(17) 0.0098(15) -0.0039(16)
C50 0.0257(19) 0.041(2) 0.036(2) 0.0001(17) 0.0084(16) 0.0028(16)
C56 0.0175(17) 0.038(2) 0.037(2) -0.0047(17) 0.0090(15) -0.0007(15)
C58 0.0260(19) 0.040(2) 0.029(2) -0.0086(16) 0.0117(15) 0.0008(16)
C59 0.038(2) 0.072(3) 0.037(3) -0.024(2) 0.0168(19) -0.018(2)
C61 0.029(2) 0.037(2) 0.045(2) -0.0115(18) 0.0161(17) -0.0010(17)
C62 0.042(2) 0.036(2) 0.059(3) 0.005(2) 0.028(2) 0.0035(19)
C63 0.053(3) 0.035(2) 0.068(3) 0.010(2) 0.033(3) 0.009(2)
C64 0.030(2) 0.042(2) 0.028(2) -0.0103(17) 0.0058(15) -0.0040(17)
O5 0.0319(15) 0.0453(17) 0.054(2) -0.0016(14) 0.0211(13) 0.0100(13)
N7 0.0330(17) 0.0263(15) 0.0272(17) 0.0006(12) 0.0155(13) 0.0037(13)
O11 0.0272(15) 0.079(2) 0.049(2) -0.0263(18) 0.0150(13) -0.0223(15)
O12 0.0322(15) 0.0587(19) 0.0338(17) -0.0073(14) 0.0194(12) -0.0098(13)
O13 0.0428(16) 0.0389(15) 0.0274(15) 0.0015(11) 0.0152(12) 0.0042(12)
N14 0.0369(18) 0.0253(15) 0.0242(16) -0.0001(12) 0.0113(13) -0.0011(13)
F2AA 0.0314(13) 0.0632(18) 0.0483(16) -0.0054(13) -0.0065(11) 0.0115(12)
F1AA 0.0463(14) 0.0452(14) 0.0344(14) 0.0087(10) 0.0053(11) 0.0062(11)
F6 0.0490(15) 0.0387(14) 0.0688(19) 0.0005(12) 0.0239(13) 0.0003(12)
F3AA 0.0264(13) 0.080(2) 0.0569(17) -0.0183(15) 0.0148(11) -0.0185(12)
C9 0.0305(19) 0.0266(18) 0.026(2) -0.0038(14) 0.0082(15) 0.0057(15)
O10 0.0620(19) 0.0304(14) 0.0225(14) -0.0036(11) 0.0077(13) -0.0106(13)
C11 0.0228(17) 0.0301(18) 0.0198(17) -0.0015(14) 0.0048(13) -0.0024(14)
C14 0.035(2) 0.0267(18) 0.0230(19) 0.0021(14) 0.0081(15) -0.0024(15)
C15 0.031(2) 0.040(2) 0.046(3) -0.0047(18) 0.0137(18) 0.0061(17)
F16 0.0672(18) 0.0481(15) 0.0479(16) 0.0070(12) 0.0381(14) -0.0061(13)
F17 0.0426(15) 0.0692(18) 0.0450(16) 0.0034(14) 0.0027(12) 0.0129(13)
O19 0.0437(17) 0.0451(17) 0.0305(15) 0.0046(12) 0.0195(12) 0.0152(13)
C20 0.040(2) 0.0286(19) 0.025(2) -0.0023(15) 0.0148(16) 0.0022(16)
C21 0.0275(19) 0.0267(18) 0.0206(17) -0.0051(14) 0.0059(14) -0.0045(14)
N22 0.0373(18) 0.0273(15) 0.0269(17) 0.0017(13) 0.0144(13) -0.0008(14)
C23 0.027(2) 0.052(3) 0.035(2) -0.0160(19) 0.0079(17) -0.0071(18)
C24 0.0317(19) 0.0261(18) 0.028(2) -0.0004(15) 0.0109(15) -0.0020(15)
C0AA 0.036(2) 0.0248(18) 0.0237(19) -0.0010(14) 0.0029(15) 0.0000(15)
C26 0.031(2) 0.075(3) 0.037(3) -0.020(2) 0.0217(18) -0.014(2)
C27 0.048(2) 0.033(2) 0.028(2) 0.0003(16) 0.0183(18) -0.0111(18)
C28 0.0216(17) 0.040(2) 0.0201(18) 0.0001(15) 0.0030(13) -0.0010(15)
C29 0.0211(17) 0.0264(18) 0.0218(18) -0.0041(13) 0.0060(13) -0.0044(13)
F1 0.0438(15) 0.0653(17) 0.0391(15) -0.0038(13) -0.0014(11) 0.0042(13)
F2 0.0661(18) 0.0299(12) 0.0583(17) -0.0087(11) 0.0249(14) -0.0216(12)
F3 0.0310(14) 0.0717(19) 0.0581(18) -0.0188(14) 0.0114(12) -0.0191(12)
F4 0.0381(14) 0.076(2) 0.0480(17) -0.0349(15) -0.0013(11) -0.0069(13)
C5 0.0264(18) 0.0270(18) 0.031(2) -0.0029(15) 0.0120(15) 0.0055(15)
C6 0.039(2) 0.0277(18) 0.0230(19) -0.0004(15) 0.0138(15) 0.0006(16)
O0AA 0.0406(16) 0.0387(15) 0.0270(15) -0.0096(11) 0.0118(12) -0.0057(12)
C2 0.025(2) 0.046(2) 0.046(3) -0.007(2) 0.0088(17) -0.0037(17)
O1 0.064(5) 0.075(6) 0.110(8) 0.015(5) -0.002(5) -0.012(4)
O1AA 0.25(2) 0.099(9) 0.45(4) 0.023(14) 0.13(2) -0.007(10)
Zn3A 0.035(3) 0.0223(15) 0.0239(9) -0.0008(9) 0.010(2) -0.003(2)
O3 0.27(3) 0.25(3) 0.27(3) 0.03(2) -0.13(2) -0.13(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
Zn1 O2 1.930(3) . ?
Zn1 N23 2.006(3) . ?
Zn1 O11 1.944(3) 3_456 ?
Zn1 N22 2.025(3) . ?
Zn2 N21 2.007(3) . ?
Zn2 C46 2.585(4) . ?
Zn2 O5 1.913(3) . ?
Zn2 N7 2.030(3) . ?
Zn2 O13 2.011(3) . ?
Zn3 N13 1.999(11) . ?
Zn3 O12 2.019(10) . ?
Zn3 N14 1.912(7) . ?
Zn3 O0AA 2.018(10) . ?
O2 C28 1.279(5) . ?
F7 C2 1.336(5) . ?
N13 C2AA 1.341(5) . ?
N13 C25 1.348(5) . ?
N13 Zn3A 1.981(11) . ?
C2AA H2AA 0.929(4) . ?
C2AA N23 1.309(5) 4_546 ?
N21 N23 1.382(4) 4_546 ?
N21 C25 1.311(5) . ?
N23 C2AA 1.309(5) 4_556 ?
N23 N21 1.382(4) 4_556 ?
F0AA C15 1.338(5) . ?
C25 H25 0.929(4) . ?
C1AA H1AA 0.931(4) . ?
C1AA C33 1.381(5) . ?
C1AA C38 1.403(5) . ?
C33 H33 0.929(4) . ?
C33 C45 1.394(6) . ?
C35 H35 0.930(4) . ?
C35 C50 1.389(6) . ?
C35 C61 1.377(6) . ?
C36 C41 1.497(5) . ?
C36 O11 1.253(5) . ?
C36 O12 1.233(5) 5_665 ?
C38 C42 1.392(5) . ?
C38 C21 1.546(5) . ?
C39 H39 0.932(4) . ?
C39 C41 1.369(6) . ?
C39 C64 1.391(6) . ?
C40 C50 1.391(6) . ?
C40 C56 1.546(5) . ?
C40 C62 1.397(6) . ?
C41 C59 1.406(6) . ?
C42 H42 0.929(4) . ?
C42 C58 1.394(6) . ?
C45 C58 1.380(6) . ?
C45 C0AA 1.499(5) . ?
C46 O75 1.245(6) . ?
C46 C61 1.497(6) . ?
C46 O5 1.274(6) . ?
C49 C56 1.544(5) . ?
C49 C64 1.390(5) . ?
C49 C26 1.392(6) . ?
C50 H50 0.932(4) . ?
C56 C15 1.535(6) . ?
C56 C2 1.547(6) . ?
C58 H58 0.930(4) . ?
C59 H59 0.930(4) . ?
C59 C26 1.378(6) . ?
C61 C63 1.383(7) . ?
C62 H62 0.932(4) . ?
C62 C63 1.382(6) . ?
C63 H63 0.929(5) . ?
C64 H64 0.932(4) . ?
N7 C20 1.321(5) . ?
N7 N22 1.384(4) 4_546 ?
O11 Zn1 1.944(3) 3_544 ?
O12 C36 1.233(5) 5_665 ?
O12 Zn3A 1.921(11) . ?
O13 H13A 0.860(3) . ?
O13 H13B 0.861(3) . ?
N14 C20 1.347(5) 4 ?
N14 C6 1.343(5) . ?
N14 Zn3A 2.214(7) . ?
F2AA C23 1.319(6) . ?
F1AA C27 1.327(5) . ?
F6 C15 1.334(5) . ?
F3AA C23 1.334(5) . ?
C9 H9 0.9300 . ?
C9 C14 1.375(5) . ?
C9 C29 1.396(5) . ?
O10 C0AA 1.258(5) . ?
C11 C14 1.395(5) . ?
C11 C28 1.484(5) . ?
C11 C5 1.387(5) . ?
C14 H14 0.9300 . ?
C15 F17 1.338(6) . ?
F16 C27 1.322(5) . ?
O19 C28 1.245(5) . ?
C20 N14 1.347(5) 4_545 ?
C20 H20 0.9300 . ?
C21 C23 1.550(5) . ?
C21 C27 1.556(5) . ?
C21 C29 1.546(5) . ?
N22 N7 1.384(4) 4_556 ?
N22 C6 1.329(5) 1_556 ?
C23 F4 1.329(5) . ?
C24 H24 0.9300 . ?
C24 C29 1.385(5) . ?
C24 C5 1.381(5) . ?
C0AA O0AA 1.260(5) . ?
C26 H26 0.9300 . ?
C27 F2 1.346(5) . ?
F1 C2 1.338(6) . ?
F3 C2 1.341(5) . ?
C5 H5 0.931(3) . ?
C6 N22 1.329(5) 1_554 ?
C6 H6 0.9300 . ?
O0AA Zn3A 1.935(10) . ?
O1 H1A 1.000(11) . ?
O1 H1B 1.003(9) . ?
O1 Zn3A 2.346(12) . ?
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
O2 Zn1 N23 127.67(12) . . ?
O2 Zn1 O11 123.95(13) . 3_456 ?
O2 Zn1 N22 97.70(12) . . ?
N23 Zn1 N22 101.73(13) . . ?
O11 Zn1 N23 97.39(14) 3_456 . ?
O11 Zn1 N22 104.24(16) 3_456 . ?
N21 Zn2 C46 105.94(13) . . ?
N21 Zn2 N7 103.67(12) . . ?
N21 Zn2 O13 105.32(12) . . ?
O5 Zn2 N21 122.13(13) . . ?
O5 Zn2 C46 28.17(15) . . ?
O5 Zn2 N7 113.58(13) . . ?
O5 Zn2 O13 112.76(13) . . ?
N7 Zn2 C46 141.52(14) . . ?
O13 Zn2 C46 99.46(14) . . ?
O13 Zn2 N7 95.82(13) . . ?
N13 Zn3 O12 102.7(4) . . ?
N13 Zn3 O0AA 124.1(5) . . ?
N14 Zn3 N13 116.0(4) . . ?
N14 Zn3 O12 99.4(4) . . ?
N14 Zn3 O0AA 102.4(4) . . ?
O0AA Zn3 O12 109.7(4) . . ?
C28 O2 Zn1 112.3(2) . . ?
C2AA N13 Zn3 125.8(4) . . ?
C2AA N13 C25 103.1(3) . . ?
C2AA N13 Zn3A 130.2(4) . . ?
C25 N13 Zn3 131.1(4) . . ?
C25 N13 Zn3A 126.1(4) . . ?
N13 C2AA H2AA 123.7(4) . . ?
N23 C2AA N13 112.9(3) 4_546 . ?
N23 C2AA H2AA 123.4(4) 4_546 . ?
N23 N21 Zn2 125.3(2) 4_546 . ?
C25 N21 Zn2 127.8(3) . . ?
C25 N21 N23 106.5(3) . 4_546 ?
C2AA N23 Zn1 132.0(3) 4_556 . ?
C2AA N23 N21 105.6(3) 4_556 4_556 ?
N21 N23 Zn1 120.7(2) 4_556 . ?
N13 C25 H25 124.2(4) . . ?
N21 C25 N13 111.9(3) . . ?
N21 C25 H25 123.9(4) . . ?
C33 C1AA H1AA 119.6(4) . . ?
C33 C1AA C38 120.8(3) . . ?
C38 C1AA H1AA 119.6(4) . . ?
C1AA C33 H33 120.0(4) . . ?
C1AA C33 C45 120.3(3) . . ?
C45 C33 H33 119.7(4) . . ?
C50 C35 H35 119.5(4) . . ?
C61 C35 H35 119.4(4) . . ?
C61 C35 C50 121.0(4) . . ?
O11 C36 C41 117.2(3) . . ?
O12 C36 C41 120.5(4) 5_665 . ?
O12 C36 O11 122.3(4) 5_665 . ?
C1AA C38 C21 119.5(3) . . ?
C42 C38 C1AA 118.0(3) . . ?
C42 C38 C21 122.5(3) . . ?
C41 C39 H39 119.4(4) . . ?
C41 C39 C64 120.9(4) . . ?
C64 C39 H39 119.7(4) . . ?
C50 C40 C56 123.3(4) . . ?
C50 C40 C62 118.3(4) . . ?
C62 C40 C56 118.2(4) . . ?
C39 C41 C36 121.3(4) . . ?
C39 C41 C59 119.4(4) . . ?
C59 C41 C36 119.1(4) . . ?
C38 C42 H42 119.3(4) . . ?
C38 C42 C58 121.1(3) . . ?
C58 C42 H42 119.6(4) . . ?
C33 C45 C0AA 119.0(3) . . ?
C58 C45 C33 119.5(3) . . ?
C58 C45 C0AA 121.4(3) . . ?
O75 C46 Zn2 77.1(3) . . ?
O75 C46 C61 121.1(4) . . ?
O75 C46 O5 122.1(4) . . ?
C61 C46 Zn2 160.4(3) . . ?
O5 C46 Zn2 45.12(19) . . ?
O5 C46 C61 116.6(4) . . ?
C64 C49 C56 123.1(3) . . ?
C64 C49 C26 118.9(4) . . ?
C26 C49 C56 117.6(4) . . ?
C35 C50 C40 120.3(4) . . ?
C35 C50 H50 119.9(4) . . ?
C40 C50 H50 119.9(4) . . ?
C40 C56 C2 106.4(3) . . ?
C49 C56 C40 111.8(3) . . ?
C49 C56 C2 112.4(3) . . ?
C15 C56 C40 111.9(3) . . ?
C15 C56 C49 106.5(3) . . ?
C15 C56 C2 107.8(3) . . ?
C42 C58 H58 120.1(4) . . ?
C45 C58 C42 120.1(3) . . ?
C45 C58 H58 119.8(4) . . ?
C41 C59 H59 120.1(4) . . ?
C26 C59 C41 119.7(4) . . ?
C26 C59 H59 120.3(4) . . ?
C35 C61 C46 120.3(4) . . ?
C35 C61 C63 119.0(4) . . ?
C63 C61 C46 120.6(4) . . ?
C40 C62 H62 119.5(4) . . ?
C63 C62 C40 120.8(4) . . ?
C63 C62 H62 119.7(4) . . ?
C61 C63 H63 119.6(5) . . ?
C62 C63 C61 120.6(4) . . ?
C62 C63 H63 119.8(5) . . ?
C39 C64 H64 120.0(4) . . ?
C49 C64 C39 120.0(4) . . ?
C49 C64 H64 119.9(4) . . ?
C46 O5 Zn2 106.7(3) . . ?
C20 N7 Zn2 128.1(3) . . ?
C20 N7 N22 106.0(3) . 4_546 ?
N22 N7 Zn2 124.0(2) 4_546 . ?
C36 O11 Zn1 123.7(3) . 3_544 ?
C36 O12 Zn3 166.0(4) 5_665 . ?
C36 O12 Zn3A 157.3(4) 5_665 . ?
Zn2 O13 H13A 110.4(2) . . ?
Zn2 O13 H13B 109.9(2) . . ?
H13A O13 H13B 108.7(3) . . ?
C20 N14 Zn3 128.1(4) 4 . ?
C20 N14 Zn3A 130.1(4) 4 . ?
C6 N14 Zn3 128.2(4) . . ?
C6 N14 C20 102.9(3) . 4 ?
C6 N14 Zn3A 125.8(4) . . ?
C14 C9 H9 119.5 . . ?
C14 C9 C29 121.1(3) . . ?
C29 C9 H9 119.5 . . ?
C14 C11 C28 120.5(3) . . ?
C5 C11 C14 118.8(3) . . ?
C5 C11 C28 120.8(3) . . ?
C9 C14 C11 120.3(3) . . ?
C9 C14 H14 119.9 . . ?
C11 C14 H14 119.9 . . ?
F0AA C15 C56 111.8(4) . . ?
F6 C15 F0AA 106.5(3) . . ?
F6 C15 C56 113.9(4) . . ?
F6 C15 F17 106.4(4) . . ?
F17 C15 F0AA 106.2(4) . . ?
F17 C15 C56 111.5(3) . . ?
N7 C20 N14 112.8(3) . 4_545 ?
N7 C20 H20 123.6 . . ?
N14 C20 H20 123.6 4_545 . ?
C38 C21 C23 112.4(3) . . ?
C38 C21 C27 106.1(3) . . ?
C23 C21 C27 108.9(3) . . ?
C29 C21 C38 111.2(3) . . ?
C29 C21 C23 106.8(3) . . ?
C29 C21 C27 111.6(3) . . ?
N7 N22 Zn1 122.7(2) 4_556 . ?
C6 N22 Zn1 130.7(3) 1_556 . ?
C6 N22 N7 105.5(3) 1_556 4_556 ?
F2AA C23 F3AA 107.4(3) . . ?
F2AA C23 C21 110.5(3) . . ?
F2AA C23 F4 107.6(4) . . ?
F3AA C23 C21 113.2(4) . . ?
F4 C23 F3AA 106.9(3) . . ?
F4 C23 C21 111.1(3) . . ?
C29 C24 H24 119.6 . . ?
C5 C24 H24 119.6 . . ?
C5 C24 C29 120.8(3) . . ?
O10 C0AA C45 119.2(3) . . ?
O10 C0AA O0AA 122.1(3) . . ?
O0AA C0AA C45 118.7(3) . . ?
C49 C26 H26 119.5 . . ?
C59 C26 C49 121.0(4) . . ?
C59 C26 H26 119.5 . . ?
F1AA C27 C21 111.0(3) . . ?
F1AA C27 F2 106.8(4) . . ?
F16 C27 F1AA 107.5(4) . . ?
F16 C27 C21 112.4(3) . . ?
F16 C27 F2 107.0(3) . . ?
F2 C27 C21 111.9(3) . . ?
O2 C28 C11 116.8(3) . . ?
O19 C28 O2 121.5(3) . . ?
O19 C28 C11 121.7(4) . . ?
C9 C29 C21 117.8(3) . . ?
C24 C29 C9 118.3(3) . . ?
C24 C29 C21 123.9(3) . . ?
C11 C5 H5 119.7(4) . . ?
C24 C5 C11 120.7(3) . . ?
C24 C5 H5 119.6(4) . . ?
N14 C6 H6 123.6 . . ?
N22 C6 N14 112.8(3) 1_554 . ?
N22 C6 H6 123.6 1_554 . ?
C0AA O0AA Zn3 103.4(3) . . ?
C0AA O0AA Zn3A 109.2(4) . . ?
F7 C2 C56 113.6(3) . . ?
F7 C2 F1 107.0(4) . . ?
F7 C2 F3 106.3(4) . . ?
F1 C2 C56 111.5(4) . . ?
F1 C2 F3 106.3(4) . . ?
F3 C2 C56 111.6(4) . . ?
H1A O1 H1B 101.6(8) . . ?
Zn3A O1 H1A 116.1(8) . . ?
Zn3A O1 H1B 116.2(7) . . ?
N13 Zn3A N14 104.4(4) . . ?
N13 Zn3A O1 79.6(4) . . ?
O12 Zn3A N13 107.1(5) . . ?
O12 Zn3A N14 92.7(4) . . ?
O12 Zn3A O0AA 117.8(5) . . ?
O12 Zn3A O1 84.4(4) . . ?
N14 Zn3A O1 175.6(6) . . ?
O0AA Zn3A N13 130.0(6) . . ?
O0AA Zn3A N14 95.0(4) . . ?
O0AA Zn3A O1 83.6(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
Zn1 O2 C28 C11 176.6(2) . . . . ?
Zn1 O2 C28 O19 -2.3(5) . . . . ?
Zn2 N21 C25 N13 173.1(3) . . . . ?
Zn2 C46 C61 C35 -27.3(12) . . . . ?
Zn2 C46 C61 C63 148.2(9) . . . . ?
Zn2 N7 C20 N14 -165.7(3) . . . 4_545 ?
Zn3 N13 C2AA N23 177.6(4) . . . 4_546 ?
Zn3 N13 C25 N21 -177.4(4) . . . . ?
Zn3 N14 C6 N22 -170.7(5) . . . 1_554 ?
C2AA N13 C25 N21 0.7(5) . . . . ?
N23 N21 C25 N13 -0.5(4) 4_546 . . . ?
C25 N13 C2AA N23 -0.6(5) . . . 4_546 ?
C1AA C33 C45 C58 -1.0(6) . . . . ?
C1AA C33 C45 C0AA -178.8(4) . . . . ?
C1AA C38 C42 C58 -1.9(6) . . . . ?
C1AA C38 C21 C23 145.8(4) . . . . ?
C1AA C38 C21 C27 -95.3(4) . . . . ?
C1AA C38 C21 C29 26.2(5) . . . . ?
C33 C1AA C38 C42 4.7(6) . . . . ?
C33 C1AA C38 C21 -177.7(4) . . . . ?
C33 C45 C58 C42 3.8(6) . . . . ?
C33 C45 C0AA O10 -30.8(5) . . . . ?
C33 C45 C0AA O0AA 146.5(4) . . . . ?
C35 C61 C63 C62 2.1(8) . . . . ?
C36 C41 C59 C26 -175.2(5) . . . . ?
C38 C1AA C33 C45 -3.2(6) . . . . ?
C38 C42 C58 C45 -2.3(6) . . . . ?
C38 C21 C23 F2AA -48.7(4) . . . . ?
C38 C21 C23 F3AA 71.7(4) . . . . ?
C38 C21 C23 F4 -168.1(3) . . . . ?
C38 C21 C27 F1AA 69.4(4) . . . . ?
C38 C21 C27 F16 -51.1(4) . . . . ?
C38 C21 C27 F2 -171.5(3) . . . . ?
C38 C21 C29 C9 47.8(4) . . . . ?
C38 C21 C29 C24 -132.7(4) . . . . ?
C39 C41 C59 C26 0.4(8) . . . . ?
C40 C56 C15 F0AA -171.8(3) . . . . ?
C40 C56 C15 F6 67.4(5) . . . . ?
C40 C56 C15 F17 -53.0(4) . . . . ?
C40 C56 C2 F7 -170.1(4) . . . . ?
C40 C56 C2 F1 68.9(4) . . . . ?
C40 C56 C2 F3 -49.8(5) . . . . ?
C40 C62 C63 C61 1.3(9) . . . . ?
C41 C36 O11 Zn1 167.1(3) . . . 3_544 ?
C41 C39 C64 C49 2.0(7) . . . . ?
C41 C59 C26 C49 2.2(8) . . . . ?
C42 C38 C21 C23 -36.6(5) . . . . ?
C42 C38 C21 C27 82.3(4) . . . . ?
C42 C38 C21 C29 -156.2(4) . . . . ?
C45 C0AA O0AA Zn3 -161.0(4) . . . . ?
C45 C0AA O0AA Zn3A -168.1(4) . . . . ?
C46 C61 C63 C62 -173.5(5) . . . . ?
O75 C46 C61 C35 176.2(5) . . . . ?
O75 C46 C61 C63 -8.3(7) . . . . ?
O75 C46 O5 Zn2 4.6(6) . . . . ?
C49 C56 C15 F0AA -49.2(5) . . . . ?
C49 C56 C15 F6 -170.1(3) . . . . ?
C49 C56 C15 F17 69.5(4) . . . . ?
C49 C56 C2 F7 67.3(5) . . . . ?
C49 C56 C2 F1 -53.8(4) . . . . ?
C49 C56 C2 F3 -172.5(3) . . . . ?
C50 C35 C61 C46 172.2(4) . . . . ?
C50 C35 C61 C63 -3.3(7) . . . . ?
C50 C40 C56 C49 -136.8(4) . . . . ?
C50 C40 C56 C15 -17.4(5) . . . . ?
C50 C40 C56 C2 100.2(5) . . . . ?
C50 C40 C62 C63 -3.5(7) . . . . ?
C56 C40 C50 C35 -171.4(4) . . . . ?
C56 C40 C62 C63 170.5(5) . . . . ?
C56 C49 C64 C39 -172.2(4) . . . . ?
C56 C49 C26 C59 170.5(5) . . . . ?
C58 C45 C0AA O10 151.5(4) . . . . ?
C58 C45 C0AA O0AA -31.3(5) . . . . ?
C61 C35 C50 C40 1.1(6) . . . . ?
C61 C46 O5 Zn2 -171.0(3) . . . . ?
C62 C40 C50 C35 2.3(6) . . . . ?
C62 C40 C56 C49 49.5(5) . . . . ?
C62 C40 C56 C15 169.0(4) . . . . ?
C62 C40 C56 C2 -73.5(5) . . . . ?
C64 C39 C41 C36 173.0(4) . . . . ?
C64 C39 C41 C59 -2.4(7) . . . . ?
C64 C49 C56 C40 -137.8(4) . . . . ?
C64 C49 C56 C15 99.6(5) . . . . ?
C64 C49 C56 C2 -18.2(6) . . . . ?
C64 C49 C26 C59 -2.6(8) . . . . ?
O5 C46 C61 C35 -8.1(6) . . . . ?
O5 C46 C61 C63 167.4(5) . . . . ?
O11 C36 C41 C39 -178.3(4) . . . . ?
O11 C36 C41 C59 -2.8(7) . . . . ?
O12 C36 C41 C39 -0.9(7) 5_665 . . . ?
O12 C36 C41 C59 174.6(5) 5_665 . . . ?
O12 C36 O11 Zn1 -10.2(7) 5_665 . . 3_544 ?
O10 C0AA O0AA Zn3 16.1(5) . . . . ?
O10 C0AA O0AA Zn3A 9.1(5) . . . . ?
C14 C9 C29 C21 -177.8(3) . . . . ?
C14 C9 C29 C24 2.7(6) . . . . ?
C14 C11 C28 O2 -6.9(5) . . . . ?
C14 C11 C28 O19 172.0(4) . . . . ?
C14 C11 C5 C24 1.8(6) . . . . ?
C15 C56 C2 F7 -49.8(5) . . . . ?
C15 C56 C2 F1 -170.9(3) . . . . ?
C15 C56 C2 F3 70.4(4) . . . . ?
C20 N14 C6 N22 -0.5(4) 4 . . 1_554 ?
C21 C38 C42 C58 -179.5(4) . . . . ?
N22 N7 C20 N14 -1.2(4) 4_546 . . 4_545 ?
C23 C21 C27 F1AA -169.4(3) . . . . ?
C23 C21 C27 F16 70.1(4) . . . . ?
C23 C21 C27 F2 -50.3(4) . . . . ?
C23 C21 C29 C9 -75.1(4) . . . . ?
C23 C21 C29 C24 104.4(4) . . . . ?
C0AA C45 C58 C42 -178.5(4) . . . . ?
C26 C49 C56 C40 49.4(5) . . . . ?
C26 C49 C56 C15 -73.2(5) . . . . ?
C26 C49 C56 C2 168.9(4) . . . . ?
C26 C49 C64 C39 0.6(7) . . . . ?
C27 C21 C23 F2AA -166.0(3) . . . . ?
C27 C21 C23 F3AA -45.6(4) . . . . ?
C27 C21 C23 F4 74.6(4) . . . . ?
C27 C21 C29 C9 166.1(3) . . . . ?
C27 C21 C29 C24 -14.4(5) . . . . ?
C28 C11 C14 C9 178.9(3) . . . . ?
C28 C11 C5 C24 -179.0(3) . . . . ?
C29 C9 C14 C11 -0.3(6) . . . . ?
C29 C21 C23 F2AA 73.4(4) . . . . ?
C29 C21 C23 F3AA -166.1(3) . . . . ?
C29 C21 C23 F4 -45.9(5) . . . . ?
C29 C21 C27 F1AA -51.9(4) . . . . ?
C29 C21 C27 F16 -172.3(3) . . . . ?
C29 C21 C27 F2 67.3(4) . . . . ?
C29 C24 C5 C11 0.5(6) . . . . ?
C5 C11 C14 C9 -1.9(6) . . . . ?
C5 C11 C28 O2 173.9(3) . . . . ?
C5 C11 C28 O19 -7.1(5) . . . . ?
C5 C24 C29 C9 -2.8(6) . . . . ?
C5 C24 C29 C21 177.8(3) . . . . ?
C2 C56 C15 F0AA 71.6(4) . . . . ?
C2 C56 C15 F6 -49.2(4) . . . . ?
C2 C56 C15 F17 -169.7(3) . . . . ?
Zn3A N13 C2AA N23 -172.2(4) . . . 4_546 ?
Zn3A N13 C25 N21 172.8(4) . . . . ?
Zn3A N14 C6 N22 -169.0(4) . . . 1_554 ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
TMPF-88.res created by SHELXL-2014/7
TITL TMPF-88 in C2/c #15
REM reset to C2/c #15
CELL 1.54178 36.4551 18.1156 14.1588 90 93.8165 90
ZERR 8 0.0009 0.0004 0.0004 0 0.0013 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H F N O Zn
UNIT 304 184 96 48 85.61 24
L.S. 12 0 0
PLAN 9
SIZE 0.02 0.12 0.2
TEMP 23
BOND
fmap 2 53
MORE -1
BOND $H
CONF
acta
REM
REM
REM
WGHT 0.117000
FVAR 0.03415
ZN1 6 0.208712 0.892196 1.066137 11.00000 0.02717 0.02581 =
0.01903 -0.00252 0.00820 -0.00378
ZN2 6 0.316493 0.344356 0.199007 11.00000 0.03147 0.02339 =
0.02816 -0.00095 0.01342 0.00560
PART 1
ZN3 6 0.318734 0.676691 0.231200 10.50000 0.02572 0.01856 =
0.02045 -0.00087 0.01037 0.00275
PART 0
O2 5 0.243203 0.896132 0.968620 11.00000 0.03402 0.03578 =
0.02915 -0.00025 0.01532 -0.00453
F7 3 0.509377 0.093698 -0.133000 11.00000 0.04063 0.05051 =
0.05018 -0.02256 0.01580 -0.00617
N13 4 0.314153 0.568972 0.258689 11.00000 0.04206 0.02538 =
0.02057 0.00124 0.01224 0.00328
C2AA 1 0.299639 0.539682 0.334800 11.00000 0.05363 0.02320 =
0.02180 -0.00081 0.01547 0.00498
H2AA 2 10.291101 10.567600 10.383801 11.00000 10.03900
N21 4 0.314148 0.447515 0.250025 11.00000 0.03171 0.02440 =
0.02101 -0.00088 0.01047 0.00508
N23 4 0.201138 0.967441 1.166977 11.00000 0.04030 0.02478 =
0.02063 -0.00081 0.00975 -0.00261
F0AA 3 0.550420 0.075701 0.028117 11.00000 0.04246 0.06012 =
0.07042 0.00349 0.02407 0.02316
C25 1 0.322973 0.509104 0.208451 11.00000 0.03756 0.02420 =
0.02206 -0.00109 0.00977 0.00136
H25 2 10.334000 10.511101 10.151201 11.00000 10.03300
C1AA 1 0.315479 0.897199 0.568919 11.00000 0.02374 0.03332 =
0.02457 -0.00572 0.00799 -0.00300
H1AA 2 10.295800 10.915100 10.600801 11.00000 10.03200
C33 1 0.310215 0.837973 0.508091 11.00000 0.02633 0.03259 =
0.03193 -0.00467 0.00710 -0.01033
H33 2 10.287499 10.814600 10.501700 11.00000 10.03600
C35 1 0.428302 0.228148 0.156577 11.00000 0.02764 0.03855 =
0.03716 -0.00366 0.01737 -0.00202
H35 2 10.415900 10.209399 10.206599 11.00000 10.04100
C36 1 0.645166 0.329656 -0.029196 11.00000 0.02826 0.03457 =
0.02979 -0.00567 0.01195 -0.00234
C38 1 0.350109 0.930706 0.583258 11.00000 0.02800 0.02677 =
0.01852 -0.00204 0.00456 -0.00348
C39 1 0.592291 0.257526 -0.102955 11.00000 0.03012 0.04000 =
0.02687 -0.00569 0.01082 -0.00059
H39 2 10.604000 10.257000 9.840500 11.00000 10.03800
C40 1 0.477356 0.217688 0.051228 11.00000 0.01943 0.03787 =
0.03559 -0.00534 0.00755 -0.00326
C41 1 0.607790 0.295736 -0.026996 11.00000 0.02008 0.04493 =
0.03705 -0.01021 0.01164 -0.00428
C42 1 0.378185 0.906046 0.529203 11.00000 0.02475 0.04135 =
0.02632 -0.00767 0.00896 -0.00601
H42 2 10.401100 10.928600 10.536200 11.00000 10.03600
C45 1 0.338906 0.812836 0.456166 11.00000 0.03415 0.02469 =
0.01691 -0.00096 0.00279 0.00094
C46 1 0.381885 0.329234 0.141317 11.00000 0.03662 0.04326 =
0.04423 -0.01200 0.01347 0.00383
O75 5 0.372059 0.390247 0.108030 11.00000 0.06102 0.04607 =
0.09381 0.00887 0.04293 0.02192
C49 1 0.541179 0.221780 -0.013696 11.00000 0.02041 0.03885 =
0.03404 -0.00670 0.00984 -0.00389
C50 1 0.458121 0.189776 0.125006 11.00000 0.02567 0.04050 =
0.03646 0.00012 0.00840 0.00285
H50 2 10.465301 10.145201 10.153400 11.00000 10.04100
C56 1 0.507267 0.173629 0.003134 11.00000 0.01750 0.03768 =
0.03729 -0.00469 0.00902 -0.00072
C58 1 0.372452 0.848314 0.464817 11.00000 0.02603 0.04033 =
0.02900 -0.00859 0.01165 0.00081
H58 2 10.391201 10.833700 10.427500 11.00000 10.03700
C59 1 0.589430 0.298795 0.057116 11.00000 0.03759 0.07158 =
0.03663 -0.02394 0.01680 -0.01838
H59 2 10.599700 10.324700 10.109100 11.00000 10.05800
C61 1 0.416777 0.293553 0.114855 11.00000 0.02872 0.03691 =
0.04531 -0.01146 0.01611 -0.00099
C62 1 0.466680 0.286011 0.012762 11.00000 0.04212 0.03598 =
0.05870 0.00546 0.02795 0.00355
H62 2 10.480100 10.306900 9.965800 11.00000 10.05300
C63 1 0.436550 0.322888 0.043698 11.00000 0.05331 0.03517 =
0.06841 0.00999 0.03282 0.00949
H63 2 10.429500 10.367801 10.016600 11.00000 10.06100
C64 1 0.559380 0.219502 -0.096811 11.00000 0.03035 0.04159 =
0.02767 -0.01028 0.00577 -0.00400
H64 2 10.549500 10.192500 9.851501 11.00000 10.04000
O5 5 0.361895 0.291974 0.194391 11.00000 0.03188 0.04528 =
0.05363 -0.00159 0.02110 0.00998
N7 4 0.278003 0.289212 0.268544 11.00000 0.03298 0.02631 =
0.02719 0.00060 0.01553 0.00375
O11 5 0.657677 0.362096 0.044226 11.00000 0.02715 0.07868 =
0.04860 -0.02633 0.01495 -0.02230
O12 5 0.336985 0.677019 0.099651 11.00000 0.03217 0.05868 =
0.03380 -0.00726 0.01943 -0.00978
O13 5 0.287466 0.346979 0.073170 11.00000 0.04277 0.03888 =
0.02745 0.00154 0.01516 0.00417
H13A 2 10.267200 10.323001 10.076099 11.00000 10.05400
H13B 2 10.300000 10.327101 10.030399 11.00000 10.05400
N14 4 0.273603 0.729154 0.206621 11.00000 0.03693 0.02533 =
0.02420 -0.00005 0.01127 -0.00114
F2AA 3 0.402653 0.928774 0.739687 11.00000 0.03141 0.06321 =
0.04827 -0.00544 -0.00653 0.01151
F1AA 3 0.315635 1.075549 0.563322 11.00000 0.04629 0.04518 =
0.03443 0.00867 0.00535 0.00623
F6 3 0.496310 0.054879 0.072193 11.00000 0.04896 0.03873 =
0.06876 0.00046 0.02390 0.00026
F3AA 3 0.420630 1.015250 0.651062 11.00000 0.02643 0.07956 =
0.05695 -0.01829 0.01480 -0.01846
C9 1 0.323147 0.921964 0.776145 11.00000 0.03049 0.02665 =
0.02562 -0.00381 0.00821 0.00567
AFIX 43
H9 2 0.337536 0.882152 0.759812 11.00000 -1.20000
AFIX 0
O10 5 0.308998 0.700852 0.408140 11.00000 0.06203 0.03042 =
0.02249 -0.00362 0.00770 -0.01056
C11 1 0.276279 0.971989 0.869067 11.00000 0.02282 0.03010 =
0.01978 -0.00149 0.00484 -0.00244
C14 1 0.297959 0.912796 0.843317 11.00000 0.03497 0.02672 =
0.02298 0.00207 0.00806 -0.00236
AFIX 43
H14 2 0.295372 0.866954 0.871683 11.00000 -1.20000
AFIX 0
C15 1 0.521281 0.107850 0.063631 11.00000 0.03134 0.04043 =
0.04574 -0.00467 0.01366 0.00613
F16 3 0.370888 1.068309 0.522460 11.00000 0.06723 0.04813 =
0.04786 0.00701 0.03811 -0.00607
F17 3 0.532187 0.128879 0.151638 11.00000 0.04259 0.06917 =
0.04502 0.00337 0.00268 0.01293
O19 5 0.231774 1.015465 0.972042 11.00000 0.04369 0.04514 =
0.03053 0.00463 0.01947 0.01523
C20 1 0.252635 0.243015 0.233166 11.00000 0.03979 0.02863 =
0.02478 -0.00230 0.01477 0.00219
AFIX 43
H20 2 0.252870 0.222288 0.173117 11.00000 -1.20000
AFIX 0
C21 1 0.355389 0.994965 0.654765 11.00000 0.02750 0.02674 =
0.02064 -0.00506 0.00586 -0.00452
N22 4 0.232478 0.808413 1.142547 11.00000 0.03730 0.02726 =
0.02687 0.00168 0.01436 -0.00084
C23 1 0.394218 0.995104 0.706592 11.00000 0.02720 0.05165 =
0.03529 -0.01596 0.00787 -0.00711
C24 1 0.306808 1.049219 0.760509 11.00000 0.03171 0.02612 =
0.02789 -0.00045 0.01090 -0.00200
AFIX 43
H24 2 0.310067 1.095512 0.733938 11.00000 -1.20000
AFIX 0
C0AA 1 0.332108 0.749363 0.389385 11.00000 0.03588 0.02479 =
0.02371 -0.00104 0.00294 0.00002
C26 1 0.556256 0.263034 0.062204 11.00000 0.03069 0.07541 =
0.03652 -0.02024 0.02174 -0.01364
AFIX 43
H26 2 0.543754 0.266521 0.117184 11.00000 -1.20000
AFIX 0
C27 1 0.350359 1.067239 0.595965 11.00000 0.04769 0.03311 =
0.02771 0.00031 0.01827 -0.01105
C28 1 0.248585 0.962073 0.940278 11.00000 0.02157 0.03962 =
0.02013 0.00009 0.00297 -0.00100
C29 1 0.327465 0.990056 0.732081 11.00000 0.02107 0.02637 =
0.02177 -0.00407 0.00597 -0.00439
F1 3 0.480578 0.196661 -0.152664 11.00000 0.04382 0.06532 =
0.03907 -0.00382 -0.00144 0.00424
F2 3 0.359248 1.127498 0.648170 11.00000 0.06610 0.02992 =
0.05834 -0.00872 0.02488 -0.02162
F3 3 0.456952 0.108660 -0.075616 11.00000 0.03095 0.07170 =
0.05805 -0.01878 0.01138 -0.01906
F4 3 0.395802 1.041399 0.779578 11.00000 0.03811 0.07580 =
0.04798 -0.03494 -0.00129 -0.00686
C5 1 0.281433 1.040339 0.827806 11.00000 0.02637 0.02697 =
0.03093 -0.00285 0.01203 0.00553
H5 2 10.267600 11.080600 10.845500 11.00000 10.03300
C6 1 0.263264 0.771097 0.131259 11.00000 0.03881 0.02769 =
0.02299 -0.00041 0.01378 0.00058
AFIX 43
H6 2 0.276254 0.773736 0.077013 11.00000 -1.20000
AFIX 0
O0AA 5 0.348743 0.747954 0.314230 11.00000 0.04059 0.03874 =
0.02699 -0.00956 0.01180 -0.00568
C2 1 0.488742 0.142784 -0.090146 11.00000 0.02474 0.04553 =
0.04594 -0.00749 0.00880 -0.00368
PART 2
O1 5 0.385976 0.619625 0.250237 10.50000 0.06359 0.07480 =
0.10977 0.01521 -0.00166 -0.01156
H1A 2 10.395201 10.608201 10.316700 10.50000 10.12100
H1B 2 10.406699 10.649900 10.227600 10.50000 10.12100
PART 0
O1AA 5 0.589945 0.528342 0.382712 0.70118 0.25337 0.09851 =
0.45067 0.02319 0.13066 -0.00730
PART 2
ZN3A 6 0.327213 0.672546 0.231165 10.50000 0.03480 0.02235 =
0.02388 -0.00080 0.01031 -0.00288
PART 0
O3 5 0.386150 0.525467 0.416990 10.50000 0.27230 0.25258 =
0.27348 0.03108 -0.13062 -0.12536
HKLF 4
REM TMPF-88 in C2/c #15
REM R1 = 0.0406 for 6378 Fo > 4sig(Fo) and 0.0517 for all 7787 data
REM 650 parameters refined using 0 restraints
END
WGHT 0.1148 0.0000
REM Highest difference peak 0.656, deepest hole -0.689, 1-sigma level 0.138
Q1 1 0.4091 0.5990 0.3232 11.00000 0.05 0.66
Q2 1 0.5319 0.5394 0.3742 11.00000 0.05 0.64
Q3 1 0.5000 0.5000 0.0000 10.50000 0.05 0.62
Q4 1 0.3787 0.5350 0.4298 11.00000 0.05 0.61
Q5 1 0.5303 0.5338 0.4970 11.00000 0.05 0.59
Q6 1 0.4220 0.4767 0.4546 11.00000 0.05 0.57
Q7 1 0.4441 0.4924 0.3751 11.00000 0.05 0.56
Q8 1 0.4372 0.5604 0.2365 11.00000 0.05 0.56
Q9 1 0.5244 0.4876 0.3685 11.00000 0.05 0.55
REM The information below was added by Olex2.
REM
REM R1 = 0.0406 for 6378 Fo > 4sig(Fo) and 0.0517 for all 38870 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.66, deepest hole -0.69
REM Mean Shift 0, Max Shift -0.010.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0517
REM R1_gt = 0.0406
REM wR_ref = 0.1593
REM GOOF = 1.064
REM Shift_max = -0.010
REM Shift_mean = 0
REM Reflections_all = 38870
REM Reflections_gt = 6378
REM Parameters = n/a
REM Hole = -0.69
REM Peak = 0.66
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1429139'
_audit_update_record
;
2015-11-24 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_audit_creation_date 2015-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic TMPF-91
_chemical_formula_moiety 'C21 H14 F6 N6 O5 Zn2'
_chemical_formula_sum 'C21 H14 F6 N6 O5 Zn2'
_chemical_formula_weight 675.12
_chemical_absolute_configuration ?
_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 0.0180 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0730 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0490 0.0320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5490 0.6780 '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 9
_space_group_name_H-M_alt 'C 1 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'
_cell_length_a 10.0888(4)
_cell_length_b 33.8241(11)
_cell_length_c 7.0903(2)
_cell_angle_alpha 90
_cell_angle_beta 96.002(2)
_cell_angle_gamma 90
_cell_volume 2406.26(14)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3338
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 64.93
_cell_measurement_theta_min 2.61
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.328
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier ?
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.864
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1344
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.02
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0449
_diffrn_reflns_av_unetI/netI 0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 39
_diffrn_reflns_limit_k_min -39
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 6938
_diffrn_reflns_point_group_measured_fraction_full 0.805
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 65.179
_diffrn_reflns_theta_min 2.613
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.956
_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 0.773
_reflns_Friedel_fraction_full 0.705
_reflns_Friedel_fraction_max 0.746
_reflns_number_gt 3143
_reflns_number_total 3504
_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 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'Bruker APEX-II CCD'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max 0.751
_refine_diff_density_min -0.677
_refine_diff_density_rms 0.177
_refine_ls_abs_structure_details
;
Flack x determined using 1253 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.02(3)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.182
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 3504
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0514
_refine_ls_R_factor_gt 0.0406
_refine_ls_restrained_S_all 1.182
_refine_ls_shift/su_max 0.030
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0796P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1120
_refine_ls_wR_factor_ref 0.1438
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Others
Fixed Uiso: H3(0.03) H18(0.034) H27(0.033) H33(0.041) H34(0.032) H37(0.034)
H38(0.039) H40(0.038) H42(0.029) H3A(0.055) H3B(0.055) H5(0.029) H9(0.047)
H1AA(0.033)
Fixed X: H3(-0.4661) H18(-0.1216) H27(-0.4024) H33(-0.222401) H34(-0.4553)
H37(-0.349699) H38(0.0049) H40(-0.0412) H42(-0.1037) H3A(-0.654) H3B(-0.5383)
H5(0.0828) H9(-0.2473) H1AA(0.1245)
Fixed Y: H3(-0.520801) H18(-0.2075) H27(-0.3571) H33(-0.2192) H34(-0.5751)
H37(-0.306399) H38(-0.3543) H40(-0.4023) H42(-0.2681) H3A(-0.566601) H3B(-
0.5879) H5(-0.4305) H9(-0.158699) H1AA(-0.473)
Fixed Z: H3(-0.118999) H18(-0.44) H27(-0.571699) H33(-1.090601) H34(-0.5917)
H37(-0.7665) H38(-0.806) H40(-0.5916) H42(-0.588799) H3A(0.0432) H3B(0.0143)
H5(-0.0913) H9(-0.946799) H1AA(0.418301)
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.18508(14) -0.47972(4) -0.17199(17) 0.0206(4) Uani 1 1 d . . . . .
Zn2 Zn -0.67171(14) -0.58484(4) -0.29290(17) 0.0216(4) Uani 1 1 d . . . . .
N2 N -0.3286(10) -0.5180(3) -0.2933(12) 0.0227(19) Uani 1 1 d . . . . .
C3 C -0.4383(12) -0.5298(3) -0.2325(17) 0.025(2) Uani 1 1 d . . . . .
H3 H -0.4661 -0.5208 -0.1190 0.030 Uiso 1 1 d . . . . .
F4 F 0.0263(8) -0.2598(2) -1.1101(13) 0.049(2) Uani 1 1 d . . . . .
O6 O -0.3733(9) -0.4202(2) -0.3787(11) 0.0296(18) Uani 1 1 d . . . . .
F7 F -0.2048(10) -0.2782(2) -1.2809(11) 0.050(2) Uani 1 1 d . . . . .
C3AA C -0.1626(12) -0.2504(3) -0.8569(17) 0.025(3) Uani 1 1 d . . . . .
C10 C -0.2569(12) -0.4165(3) -0.4219(13) 0.020(2) Uani 1 1 d . . . . .
C2AA C -0.1661(14) -0.3248(3) -0.8097(16) 0.023(2) Uani 1 1 d . . . . .
F12 F 0.0905(7) -0.2899(2) -0.8521(11) 0.0415(18) Uani 1 1 d . . . . .
F15 F -0.3601(8) -0.2885(3) -1.1073(11) 0.0479(19) Uani 1 1 d . . . . .
O16 O -0.1594(9) -0.4386(2) -0.3591(12) 0.034(2) Uani 1 1 d . . . . .
C17 C -0.2360(15) -0.2986(4) -1.1247(18) 0.034(3) Uani 1 1 d . . . . .
C18 C -0.1420(13) -0.2097(4) -0.5707(15) 0.029(3) Uani 1 1 d . . . . .
H18 H -0.1216 -0.2075 -0.4400 0.034 Uiso 1 1 d . . . . .
F19 F -0.2397(10) -0.3365(2) -1.1785(11) 0.054(2) Uani 1 1 d . . . . .
F21 F 0.0281(8) -0.3233(2) -1.1044(12) 0.0445(19) Uani 1 1 d . . . . .
C25 C -0.2259(13) -0.3844(3) -0.5592(15) 0.026(2) Uani 1 1 d . . . . .
C26 C 0.0010(14) -0.2910(3) -1.0045(18) 0.036(3) Uani 1 1 d . . . . .
C27 C -0.3185(12) -0.3562(3) -0.6148(18) 0.028(2) Uani 1 1 d . . . . .
H27 H -0.4024 -0.3571 -0.5717 0.033 Uiso 1 1 d . . . . .
N29 N -0.5090(10) -0.5554(3) -0.3428(12) 0.025(2) Uani 1 1 d . . . . .
C33 C -0.2033(14) -0.2170(4) -0.9600(16) 0.034(3) Uani 1 1 d . . . . .
H33 H -0.2224 -0.2192 -1.0906 0.041 Uiso 1 1 d . . . . .
C34 C -0.4328(13) -0.5588(3) -0.4877(16) 0.026(2) Uani 1 1 d . . . . .
H34 H -0.4553 -0.5751 -0.5917 0.032 Uiso 1 1 d . . . . .
C35 C -0.1406(12) -0.2910(3) -0.9485(15) 0.023(2) Uani 1 1 d . . . . .
C37 C -0.2872(11) -0.3262(3) -0.7350(18) 0.028(3) Uani 1 1 d . . . . .
H37 H -0.3497 -0.3064 -0.7665 0.034 Uiso 1 1 d . . . . .
C38 C -0.0770(13) -0.3539(4) -0.7565(19) 0.032(3) Uani 1 1 d . . . . .
H38 H 0.0049 -0.3543 -0.8060 0.039 Uiso 1 1 d . . . . .
C40 C -0.1052(13) -0.3833(3) -0.6294(19) 0.032(3) Uani 1 1 d . . . . .
H40 H -0.0412 -0.4023 -0.5916 0.038 Uiso 1 1 d . . . . .
C42 C -0.1315(12) -0.2461(3) -0.6610(17) 0.024(2) Uani 1 1 d . . . . .
H42 H -0.1037 -0.2681 -0.5888 0.029 Uiso 1 1 d . . . . .
N1 N -0.0354(10) -0.4662(3) 0.0361(12) 0.0226(19) Uani 1 1 d . . . . .
C2 C -0.1824(14) -0.1772(3) -0.6770(17) 0.025(2) Uani 1 1 d . . . . .
O3 O -0.6241(10) -0.5872(3) -0.0117(12) 0.036(2) Uani 1 1 d . . . . .
H3A H -0.6540 -0.5666 0.0432 0.055 Uiso 1 1 d . . . . .
H3B H -0.5383 -0.5879 0.0143 0.055 Uiso 1 1 d . . . . .
C5 C 0.0688(13) -0.4441(3) 0.0188(16) 0.024(2) Uani 1 1 d . . . . .
H5 H 0.0828 -0.4305 -0.0913 0.029 Uiso 1 1 d . . . . .
N0AA N -0.0215(11) -0.4813(3) 0.2149(14) 0.028(2) Uani 1 1 d . . . . .
O7 O -0.1801(10) -0.1375(2) -0.4044(12) 0.034(2) Uani 1 1 d . . . . .
N8 N 0.1524(9) -0.4434(3) 0.1771(14) 0.025(2) Uani 1 1 d . . . . .
C9 C -0.2165(16) -0.1805(3) -0.875(2) 0.039(3) Uani 1 1 d . . . . .
H9 H -0.2473 -0.1587 -0.9468 0.047 Uiso 1 1 d . . . . .
C1AA C 0.0902(13) -0.4673(4) 0.2943(16) 0.028(2) Uani 1 1 d . . . . .
H1AA H 0.1245 -0.4730 0.4183 0.033 Uiso 1 1 d . . . . .
C11 C -0.1924(12) -0.1371(3) -0.5837(16) 0.025(2) Uani 1 1 d . . . . .
N12 N -0.3243(9) -0.5370(3) -0.4686(12) 0.0231(19) Uani 1 1 d . . . . .
O1 O -0.2115(11) -0.1067(2) -0.6796(14) 0.039(2) 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
Zn1 0.0215(8) 0.0221(7) 0.0177(6) 0.0015(5) -0.0012(5) -0.0043(6)
Zn2 0.0204(8) 0.0208(7) 0.0236(8) -0.0005(6) 0.0023(5) -0.0005(6)
N2 0.029(6) 0.019(4) 0.021(4) 0.002(4) 0.005(4) -0.003(4)
C3 0.018(6) 0.029(5) 0.027(5) -0.005(4) 0.001(4) -0.009(4)
F4 0.041(5) 0.050(5) 0.061(5) 0.024(4) 0.021(4) -0.004(4)
O6 0.028(5) 0.034(4) 0.027(4) 0.007(3) 0.004(3) -0.001(3)
F7 0.082(7) 0.040(4) 0.027(4) 0.008(3) 0.010(4) -0.007(4)
C3AA 0.031(7) 0.019(5) 0.026(6) -0.008(4) 0.007(5) -0.007(5)
C10 0.033(7) 0.014(5) 0.012(5) 0.001(4) -0.005(4) -0.001(4)
C2AA 0.038(7) 0.017(5) 0.015(5) -0.001(4) 0.008(4) -0.001(5)
F12 0.020(4) 0.049(4) 0.054(5) 0.005(4) -0.002(3) -0.001(3)
F15 0.036(5) 0.067(5) 0.039(4) 0.005(4) -0.005(3) -0.001(4)
O16 0.035(5) 0.030(4) 0.036(5) 0.018(3) 0.008(4) 0.000(4)
C17 0.053(10) 0.027(6) 0.026(6) 0.004(5) 0.014(6) 0.003(6)
C18 0.036(8) 0.032(6) 0.019(6) -0.005(5) 0.004(5) -0.004(5)
F19 0.094(8) 0.031(4) 0.034(4) -0.009(3) -0.005(4) -0.006(4)
F21 0.036(5) 0.052(5) 0.048(4) -0.001(4) 0.021(3) 0.007(4)
C25 0.042(7) 0.017(5) 0.018(5) -0.001(4) 0.006(5) -0.005(5)
C26 0.045(9) 0.025(6) 0.039(7) 0.004(5) 0.013(6) -0.006(5)
C27 0.020(6) 0.031(6) 0.033(6) 0.007(5) 0.010(4) -0.002(5)
N29 0.031(6) 0.033(5) 0.013(4) 0.001(4) 0.003(4) 0.004(4)
C33 0.051(9) 0.027(6) 0.022(6) -0.004(5) -0.004(5) 0.004(5)
C34 0.032(7) 0.028(6) 0.020(5) -0.004(4) 0.005(4) -0.009(5)
C35 0.033(7) 0.019(5) 0.020(6) 0.004(4) 0.013(4) 0.005(4)
C37 0.019(6) 0.023(5) 0.042(7) 0.007(5) 0.003(5) -0.001(4)
C38 0.025(7) 0.033(6) 0.041(7) 0.000(5) 0.014(5) 0.000(5)
C40 0.028(7) 0.028(6) 0.040(7) 0.010(5) 0.006(5) 0.013(5)
C42 0.025(6) 0.023(5) 0.024(6) 0.007(4) -0.001(4) 0.005(4)
N1 0.028(5) 0.031(5) 0.009(4) -0.002(3) -0.001(3) 0.001(4)
C2 0.034(7) 0.028(5) 0.016(5) -0.003(5) 0.011(4) -0.002(5)
O3 0.035(5) 0.050(5) 0.024(4) -0.001(4) 0.000(3) -0.005(4)
C5 0.025(6) 0.028(5) 0.018(5) -0.003(4) -0.003(4) -0.004(4)
N0AA 0.029(6) 0.023(4) 0.030(5) 0.005(4) 0.002(4) -0.001(4)
O7 0.049(6) 0.026(4) 0.029(5) -0.002(3) 0.005(4) -0.003(4)
N8 0.014(5) 0.026(5) 0.034(5) -0.002(4) 0.004(4) -0.002(3)
C9 0.067(11) 0.015(6) 0.035(7) 0.004(5) -0.005(6) 0.003(6)
C1AA 0.031(7) 0.032(5) 0.019(6) 0.012(5) -0.004(4) -0.007(5)
C11 0.024(7) 0.022(6) 0.030(6) -0.003(5) 0.001(4) -0.003(4)
N12 0.027(6) 0.023(4) 0.020(4) -0.006(4) 0.005(4) -0.001(4)
O1 0.059(7) 0.019(4) 0.041(5) 0.001(4) 0.015(5) -0.002(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
Zn1 N2 2.063(10) . ?
Zn1 O16 1.957(7) . ?
Zn1 N1 2.049(9) . ?
Zn1 N0AA 2.320(10) 2_544 ?
Zn1 N12 2.190(9) 2_545 ?
Zn2 N29 1.982(10) . ?
Zn2 O3 2.003(8) . ?
Zn2 O7 1.946(8) 3_445 ?
Zn2 N8 2.007(10) 2_444 ?
N2 C3 1.291(16) . ?
N2 N12 1.404(13) . ?
C3 N29 1.326(16) . ?
F4 C26 1.333(13) . ?
O6 C10 1.250(15) . ?
F7 C17 1.370(14) . ?
C3AA C33 1.384(17) . ?
C3AA C35 1.546(14) . ?
C3AA C42 1.399(17) . ?
C10 O16 1.278(14) . ?
C10 C25 1.513(14) . ?
C2AA C35 1.547(15) . ?
C2AA C37 1.382(18) . ?
C2AA C38 1.360(18) . ?
F12 C26 1.334(16) . ?
F15 C17 1.316(16) . ?
C17 F19 1.335(14) . ?
C17 C35 1.517(18) . ?
C18 C42 1.397(16) . ?
C18 C2 1.371(17) . ?
F21 C26 1.346(15) . ?
C25 C27 1.365(18) . ?
C25 C40 1.364(18) . ?
C26 C35 1.523(18) . ?
C27 C37 1.382(16) . ?
N29 C34 1.351(15) . ?
C33 C9 1.387(17) . ?
C34 N12 1.315(15) . ?
C38 C40 1.390(17) . ?
N1 C5 1.306(16) . ?
N1 N0AA 1.360(13) . ?
C2 C9 1.416(17) . ?
C2 C11 1.516(15) . ?
C5 N8 1.332(15) . ?
N0AA Zn1 2.320(10) 2_545 ?
N0AA C1AA 1.295(16) . ?
O7 Zn2 1.946(8) 3 ?
O7 C11 1.265(15) . ?
N8 Zn2 2.007(9) 2_645 ?
N8 C1AA 1.360(15) . ?
C11 O1 1.237(15) . ?
N12 Zn1 2.190(9) 2_544 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zn1 N0AA 89.6(3) . 2_544 ?
N2 Zn1 N12 88.1(4) . 2_545 ?
O16 Zn1 N2 107.5(4) . . ?
O16 Zn1 N1 100.9(4) . . ?
O16 Zn1 N0AA 91.2(4) . 2_544 ?
O16 Zn1 N12 113.7(3) . 2_545 ?
N1 Zn1 N2 150.7(4) . . ?
N1 Zn1 N0AA 83.0(4) . 2_544 ?
N1 Zn1 N12 86.8(4) . 2_545 ?
N12 Zn1 N0AA 154.5(3) 2_545 2_544 ?
N29 Zn2 O3 94.7(4) . . ?
N29 Zn2 N8 118.8(4) . 2_444 ?
O3 Zn2 N8 104.0(4) . 2_444 ?
O7 Zn2 N29 112.8(4) 3_445 . ?
O7 Zn2 O3 111.3(4) 3_445 . ?
O7 Zn2 N8 113.1(4) 3_445 2_444 ?
C3 N2 Zn1 130.0(8) . . ?
C3 N2 N12 105.2(9) . . ?
N12 N2 Zn1 124.8(7) . . ?
N2 C3 N29 115.6(11) . . ?
C33 C3AA C35 123.4(10) . . ?
C33 C3AA C42 117.6(10) . . ?
C42 C3AA C35 118.9(11) . . ?
O6 C10 O16 124.5(9) . . ?
O6 C10 C25 119.4(10) . . ?
O16 C10 C25 116.2(11) . . ?
C37 C2AA C35 118.8(10) . . ?
C38 C2AA C35 124.2(11) . . ?
C38 C2AA C37 117.0(10) . . ?
C10 O16 Zn1 120.0(7) . . ?
F7 C17 C35 113.7(11) . . ?
F15 C17 F7 104.2(10) . . ?
F15 C17 F19 106.1(12) . . ?
F15 C17 C35 113.9(10) . . ?
F19 C17 F7 104.8(9) . . ?
F19 C17 C35 113.2(10) . . ?
C2 C18 C42 119.1(10) . . ?
C27 C25 C10 120.5(11) . . ?
C27 C25 C40 119.0(10) . . ?
C40 C25 C10 120.5(11) . . ?
F4 C26 F12 106.2(11) . . ?
F4 C26 F21 106.6(10) . . ?
F4 C26 C35 112.7(11) . . ?
F12 C26 F21 107.0(11) . . ?
F12 C26 C35 111.2(10) . . ?
F21 C26 C35 112.6(10) . . ?
C25 C27 C37 119.9(11) . . ?
C3 N29 Zn2 128.9(8) . . ?
C3 N29 C34 100.9(10) . . ?
C34 N29 Zn2 129.9(8) . . ?
C3AA C33 C9 122.3(11) . . ?
N12 C34 N29 114.1(10) . . ?
C2AA C35 C3AA 110.4(9) . . ?
C17 C35 C3AA 113.0(10) . . ?
C17 C35 C2AA 105.4(10) . . ?
C17 C35 C26 108.5(9) . . ?
C26 C35 C3AA 106.8(10) . . ?
C26 C35 C2AA 112.9(10) . . ?
C2AA C37 C27 121.9(11) . . ?
C2AA C38 C40 121.5(12) . . ?
C25 C40 C38 120.5(11) . . ?
C3AA C42 C18 121.8(10) . . ?
C5 N1 Zn1 126.8(8) . . ?
C5 N1 N0AA 107.2(10) . . ?
N0AA N1 Zn1 125.7(7) . . ?
C18 C2 C9 120.7(10) . . ?
C18 C2 C11 120.4(11) . . ?
C9 C2 C11 118.9(10) . . ?
N1 C5 N8 112.1(10) . . ?
N1 N0AA Zn1 121.8(8) . 2_545 ?
C1AA N0AA Zn1 132.5(8) . 2_545 ?
C1AA N0AA N1 105.6(9) . . ?
C11 O7 Zn2 113.3(7) . 3 ?
C5 N8 Zn2 125.0(8) . 2_645 ?
C5 N8 C1AA 102.3(10) . . ?
C1AA N8 Zn2 132.7(8) . 2_645 ?
C33 C9 C2 118.4(11) . . ?
N0AA C1AA N8 112.8(9) . . ?
O7 C11 C2 115.2(10) . . ?
O1 C11 C2 121.1(11) . . ?
O1 C11 O7 123.6(11) . . ?
N2 N12 Zn1 123.1(7) . 2_544 ?
C34 N12 Zn1 131.4(7) . 2_544 ?
C34 N12 N2 104.1(9) . . ?
_iucr_refine_instructions_details
;
TITL UNTITLED OLEX2: imported from CIF
CELL 1.54178 10.0888 33.8241 7.0903 90 96.002 90
ZERR 4 0.0004 0.0011 0.0002 0 0.002 0
LATT -7
SYMM +X,-Y,0.5+Z
SFAC C H F N O Zn
DISP C 0.018 0.009
DISP F 0.073 0.053
DISP H 0 0
DISP N 0.031 0.018
DISP O 0.049 0.032
DISP Zn -1.549 0.678
UNIT 84 56 24 24 20 8
L.S. 4 0 0
PLAN 20
TEMP 20(2)
fmap 2 53
ACTA
REM
REM
REM
WGHT 0.079600
FVAR 0.09572
ZN1 6 -0.185083 -0.479724 -0.171993 11.00000 0.02150 0.02206 =
0.01767 0.00151 -0.00117 -0.00434
ZN2 6 -0.671711 -0.584836 -0.292903 11.00000 0.02040 0.02080 =
0.02364 -0.00048 0.00235 -0.00050
N2 4 -0.328590 -0.518042 -0.293256 11.00000 0.02874 0.01893 =
0.02090 0.00170 0.00487 -0.00259
C3 1 -0.438298 -0.529773 -0.232522 11.00000 0.01812 0.02938 =
0.02663 -0.00549 0.00114 -0.00947
H3 2 9.533900 9.479199 9.881001 11.00000 10.03000
F4 3 0.026305 -0.259838 -1.110120 11.00000 0.04064 0.05020 =
0.06059 0.02447 0.02140 -0.00429
O6 5 -0.373268 -0.420162 -0.378746 11.00000 0.02778 0.03394 =
0.02739 0.00722 0.00370 -0.00125
F7 3 -0.204829 -0.278155 -1.280921 11.00000 0.08223 0.04018 =
0.02742 0.00842 0.01050 -0.00698
C3AA 1 -0.162636 -0.250397 -0.856880 11.00000 0.03137 0.01863 =
0.02591 -0.00754 0.00723 -0.00685
C10 1 -0.256920 -0.416537 -0.421932 11.00000 0.03344 0.01431 =
0.01165 0.00132 -0.00464 -0.00143
C2AA 1 -0.166140 -0.324804 -0.809717 11.00000 0.03805 0.01715 =
0.01452 -0.00116 0.00806 -0.00070
F12 3 0.090454 -0.289890 -0.852062 11.00000 0.02008 0.04906 =
0.05423 0.00484 -0.00166 -0.00096
F15 3 -0.360077 -0.288513 -1.107256 11.00000 0.03576 0.06685 =
0.03934 0.00514 -0.00452 -0.00122
O16 5 -0.159428 -0.438618 -0.359067 11.00000 0.03511 0.03046 =
0.03613 0.01769 0.00845 0.00008
C17 1 -0.235965 -0.298625 -1.124723 11.00000 0.05327 0.02667 =
0.02553 0.00429 0.01430 0.00260
C18 1 -0.141983 -0.209673 -0.570664 11.00000 0.03593 0.03174 =
0.01869 -0.00513 0.00411 -0.00367
H18 2 9.878400 9.792500 9.560000 11.00000 10.03400
F19 3 -0.239655 -0.336468 -1.178483 11.00000 0.09409 0.03108 =
0.03396 -0.00897 -0.00525 -0.00591
F21 3 0.028058 -0.323318 -1.104426 11.00000 0.03641 0.05239 =
0.04845 -0.00109 0.02146 0.00693
C25 1 -0.225943 -0.384415 -0.559212 11.00000 0.04232 0.01687 =
0.01811 -0.00058 0.00637 -0.00467
C26 1 0.001039 -0.291011 -1.004480 11.00000 0.04505 0.02481 =
0.03914 0.00425 0.01336 -0.00578
C27 1 -0.318542 -0.356178 -0.614845 11.00000 0.02048 0.03100 =
0.03265 0.00669 0.00976 -0.00162
H27 2 9.597600 9.642900 9.428301 11.00000 10.03300
N29 4 -0.509031 -0.555431 -0.342821 11.00000 0.03084 0.03281 =
0.01271 0.00082 0.00335 0.00353
C33 1 -0.203279 -0.217028 -0.960024 11.00000 0.05085 0.02693 =
0.02224 -0.00390 -0.00411 0.00371
H33 2 9.777599 9.780800 8.909399 11.00000 10.04100
C34 1 -0.432800 -0.558797 -0.487666 11.00000 0.03239 0.02761 =
0.01977 -0.00360 0.00526 -0.00922
H34 2 9.544700 9.424900 9.408300 11.00000 10.03200
C35 1 -0.140644 -0.291033 -0.948473 11.00000 0.03289 0.01861 =
0.02014 0.00449 0.01275 0.00528
C37 1 -0.287240 -0.326179 -0.734953 11.00000 0.01891 0.02347 =
0.04183 0.00708 0.00340 -0.00115
H37 2 9.650301 9.693601 9.233500 11.00000 10.03400
C38 1 -0.077040 -0.353925 -0.756542 11.00000 0.02525 0.03273 =
0.04095 0.00014 0.01375 0.00004
H38 2 10.004900 9.645700 9.194000 11.00000 10.03900
C40 1 -0.105205 -0.383270 -0.629396 11.00000 0.02764 0.02788 =
0.03978 0.00996 0.00612 0.01347
H40 2 9.958800 9.597700 9.408400 11.00000 10.03800
C42 1 -0.131527 -0.246083 -0.660958 11.00000 0.02463 0.02338 =
0.02376 0.00743 -0.00120 0.00506
H42 2 9.896300 9.731900 9.411201 11.00000 10.02900
N1 4 -0.035369 -0.466229 0.036082 11.00000 0.02754 0.03106 =
0.00858 -0.00199 -0.00119 0.00052
C2 1 -0.182445 -0.177181 -0.677042 11.00000 0.03443 0.02763 =
0.01620 -0.00319 0.01095 -0.00204
O3 5 -0.624101 -0.587228 -0.011721 11.00000 0.03486 0.04986 =
0.02402 -0.00148 -0.00038 -0.00530
H3A 2 9.346000 9.433399 10.043200 11.00000 10.05500
H3B 2 9.461700 9.412100 10.014300 11.00000 10.05500
C5 1 0.068833 -0.444122 0.018769 11.00000 0.02489 0.02779 =
0.01811 -0.00261 -0.00269 -0.00376
H5 2 10.082800 9.569500 9.908700 11.00000 10.02900
N0AA 4 -0.021500 -0.481266 0.214947 11.00000 0.02936 0.02332 =
0.03029 0.00470 0.00168 -0.00076
O7 5 -0.180116 -0.137482 -0.404354 11.00000 0.04901 0.02563 =
0.02862 -0.00225 0.00539 -0.00279
N8 4 0.152379 -0.443386 0.177108 11.00000 0.01447 0.02599 =
0.03422 -0.00242 0.00445 -0.00183
C9 1 -0.216481 -0.180473 -0.875338 11.00000 0.06670 0.01483 =
0.03459 0.00384 -0.00519 0.00318
H9 2 9.752700 9.841301 9.053201 11.00000 10.04700
C1AA 1 0.090249 -0.467327 0.294344 11.00000 0.03099 0.03209 =
0.01886 0.01180 -0.00436 -0.00715
H1AA 2 10.124500 9.527000 10.418301 11.00000 10.03300
C11 1 -0.192356 -0.137117 -0.583723 11.00000 0.02413 0.02168 =
0.02961 -0.00252 0.00059 -0.00323
N12 4 -0.324273 -0.537002 -0.468627 11.00000 0.02726 0.02264 =
0.01989 -0.00609 0.00455 -0.00084
O1 5 -0.211482 -0.106715 -0.679593 11.00000 0.05889 0.01868 =
0.04079 0.00076 0.01475 -0.00231
HKLF 4
REM UNTITLED OLEX2: imported from CIF
REM R1 = 0.0406 for 3143 Fo > 4sig(Fo) and 0.0514 for all 3504 data
REM 361 parameters refined using 2 restraints
END
WGHT 0.0793 0.0000
REM Highest difference peak 0.751, deepest hole -0.677, 1-sigma level 0.177
Q1 1 -0.2607 -0.4974 -0.2365 11.00000 0.05 0.75
Q2 1 0.0718 -0.3836 -0.3819 11.00000 0.05 0.70
Q3 1 -0.4203 -0.4000 -0.3264 11.00000 0.05 0.68
Q4 1 -0.6009 -0.5586 -0.2462 11.00000 0.05 0.64
Q5 1 -0.1051 -0.1791 -0.2800 11.00000 0.05 0.60
Q6 1 -0.0977 -0.5025 0.2713 11.00000 0.05 0.59
Q7 1 0.2415 -0.4419 0.2352 11.00000 0.05 0.59
Q8 1 -0.0822 -0.1612 -0.6665 11.00000 0.05 0.57
Q9 1 -0.0956 -0.4614 -0.1093 11.00000 0.05 0.56
Q10 1 0.0628 -0.3946 -0.2536 11.00000 0.05 0.55
Q11 1 -0.2681 -0.3943 -0.7940 11.00000 0.05 0.55
Q12 1 -0.2563 -0.1756 -0.2831 11.00000 0.05 0.54
Q13 1 -0.0930 -0.3818 -0.7785 11.00000 0.05 0.53
Q14 1 -0.4217 -0.4428 -0.3441 11.00000 0.05 0.51
Q15 1 -0.5778 -0.6012 0.1804 11.00000 0.05 0.51
Q16 1 -0.4386 -0.2981 -1.2793 11.00000 0.05 0.50
Q17 1 -0.4190 -0.5420 -0.1251 11.00000 0.05 0.50
Q18 1 0.0623 -0.4597 0.1348 11.00000 0.05 0.50
Q19 1 0.0840 -0.2989 -1.3065 11.00000 0.05 0.49
Q20 1 -0.2397 -0.1820 -0.4222 11.00000 0.05 0.48
REM The information below was added by Olex2.
REM
REM R1 = 0.0406 for 3143 Fo > 4sig(Fo) and 0.0514 for all 7014 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.75, deepest hole -0.68
REM Mean Shift 0.006, Max Shift 0.030.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0514
REM R1_gt = 0.0406
REM wR_ref = 0.1438
REM GOOF = 1.182
REM Shift_max = 0.030
REM Shift_mean = 0.006
REM Reflections_all = 7014
REM Reflections_gt = 3143
REM Parameters = n/a
REM Hole = -0.68
REM Peak = 0.75
REM Flack = 0.02(3)
;
_olex2_submission_original_sample_id TMPF-91
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_TMPF-95
_database_code_depnum_ccdc_archive 'CCDC 1429140'
_audit_update_record
;
2015-11-24 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_TMPF-95
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 217 Ang3
RESPONSE: This is a porous Metal-Organic Framework
;
_audit_creation_date 2015-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014-3
_chemical_name_common ?
_chemical_name_systematic TMPF-95
_chemical_formula_moiety 'C72 H38 Co5 F24 N6 O17, 0.48(O)'
_chemical_formula_sum 'C72 H38 Co5 F24 N6 O17.48'
_chemical_formula_weight 2017.37
_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'
Co Co -2.3653 3.6143 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.8692(5)
_cell_length_b 24.8713(8)
_cell_length_c 22.1361(7)
_cell_angle_alpha 90
_cell_angle_beta 91.621(2)
_cell_angle_gamma 90
_cell_volume 8183.0(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 7289
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 65.223
_cell_measurement_theta_min 2.672
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 8.887
_exptl_absorpt_correction_T_max 0.7526
_exptl_absorpt_correction_T_min 0.4923
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1361 before and 0.0884 after correction.
The Ratio of minimum to maximum transmission is 0.6541.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour pink
_exptl_crystal_density_diffrn 1.638
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 4011
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.04
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1282
_diffrn_reflns_av_unetI/netI 0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 62029
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 65.880
_diffrn_reflns_theta_min 2.673
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.971
_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 8518
_reflns_number_total 13811
_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 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'Bruker APEX-II CCD'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.867
_refine_diff_density_min -0.730
_refine_diff_density_rms 0.132
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1202
_refine_ls_number_reflns 13811
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.1298
_refine_ls_R_factor_gt 0.0776
_refine_ls_restrained_S_all 1.013
_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^)+(0.1413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1994
_refine_ls_wR_factor_ref 0.2400
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C2 \\sim C7 \\sim C3: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Others
Sof(C108)=Sof(H108)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C400)=Sof(H400)=1-
FVAR(1)
Sof(C1)=Sof(H1)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=FVAR(1)
Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C7)=Sof(H7)=Sof(C9)=Sof(H9)=1-FVAR(2)
Sof(C110)=Sof(H110)=Sof(C113)=Sof(H113)=Sof(C17)=Sof(H17)=Sof(C19)=Sof(H19)=
FVAR(2)
4.a Rotating group:
O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
C26(H26), C36(H36), C39(H39), C55(H55), C57(H57), C59(H59), C60(H60),
C61(H61), C67(H67), C69(H69), C70(H70), C71(H71), C74(H74), C75(H75), C77(H77),
C83(H83), C85(H85), C86(H86), C87(H87), C89(H89), C93(H93), C97(H97),
C99(H99), C100(H100), C104(H104), C106(H106), C108(H108), C110(H110),
C113(H113), C8(H8), C0AA(H0AA), C13(H13), C14(H14), C17(H17), C19(H19), C1(H1),
C2(H2), C3(H3), C4(H4), C5(H5), C400(H400), C6(H6), C7(H7), C9(H9)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.52149(7) 0.38165(5) 0.50160(5) 0.0216(3) Uani 1 1 d . . . . .
Co2 Co 0.67827(7) 0.47268(4) 0.74405(5) 0.0212(3) Uani 1 1 d . . . . .
Co3 Co 1.48454(8) 0.32065(5) 0.35390(5) 0.0238(3) Uani 1 1 d . . . . .
Co4 Co 0.79202(8) 0.21705(4) 0.75046(5) 0.0227(3) Uani 1 1 d . . . . .
Co5 Co 0.68822(7) 0.33181(4) 0.74909(5) 0.0214(3) Uani 1 1 d . . . . .
F2 F 0.4355(3) 0.3341(2) 1.0850(2) 0.0468(13) Uani 1 1 d . . . . .
O1AA O 1.4160(4) 0.6194(2) 0.6424(2) 0.0342(13) Uani 1 1 d . . . . .
O4 O 0.7510(3) 0.2715(2) 0.8133(2) 0.0301(12) Uani 1 1 d . . . . .
O3AA O 0.6134(4) 0.3638(2) 0.8137(2) 0.0315(12) Uani 1 1 d . . . . .
O6 O 1.4038(4) 0.3524(3) 0.4210(3) 0.0470(16) Uani 1 1 d . . . . .
O8 O 0.5985(3) 0.2711(2) 0.7295(2) 0.0307(12) Uani 1 1 d . . . . .
O10 O 1.3846(4) 0.2590(2) 0.3356(2) 0.0347(13) Uani 1 1 d . . . . .
F12 F 0.4660(3) 0.4182(2) 1.0937(2) 0.0467(13) Uani 1 1 d . . . . .
O13 O 1.4184(4) 0.5726(2) 0.5559(3) 0.0407(14) Uani 1 1 d . . . . .
O14 O 1.5625(4) 0.3078(2) 0.5054(2) 0.0372(14) Uani 1 1 d . . . . .
F15 F 0.2381(4) 0.4616(2) 0.9940(3) 0.0592(15) Uani 1 1 d . . . . .
F16 F 0.3545(4) 0.3853(2) 1.1393(2) 0.0594(16) Uani 1 1 d . . . . .
F17 F 0.3305(4) 0.4871(2) 1.0643(3) 0.0524(14) Uani 1 1 d . . . . .
O18 O 1.5536(4) 0.2735(2) 0.4108(3) 0.0384(14) Uani 1 1 d . . . . .
F19 F 1.2676(4) 0.4166(3) 0.8222(3) 0.0683(17) Uani 1 1 d . . . . .
N20 N 1.4125(4) 0.3725(3) 0.2952(3) 0.0291(15) Uani 1 1 d . . . . .
F21 F 0.9401(4) 0.4600(3) 0.4655(4) 0.0716(19) Uani 1 1 d . . . . .
O22 O 1.3921(4) 0.3993(3) 0.5044(3) 0.0431(15) Uani 1 1 d . . . . .
F23 F 1.1850(5) 0.3008(2) 0.7046(3) 0.076(2) Uani 1 1 d . . . . .
N25 N 0.6579(4) 0.5516(2) 0.7316(3) 0.0255(14) Uani 1 1 d . . . . .
C26 C 0.7117(5) 0.5943(3) 0.7432(4) 0.0283(17) Uani 1 1 d . . . . .
H26 H 0.7696 0.5915 0.7600 0.034 Uiso 1 1 calc R . . . .
N27 N 0.8266(4) 0.1405(2) 0.7720(3) 0.0233(13) Uani 1 1 d . . . . .
O28 O 0.6723(4) 0.1936(2) 0.7205(3) 0.0481(17) Uani 1 1 d . . . . .
O29 O 0.8932(4) 0.2436(2) 0.6965(3) 0.0376(14) Uani 1 1 d . . . . .
F30 F 1.1872(4) 0.3527(2) 0.6270(3) 0.0581(15) Uani 1 1 d . . . . .
O31 O 0.7703(4) 0.2921(3) 0.6858(3) 0.0443(15) Uani 1 1 d . . . . .
F33 F 0.2204(4) 0.4362(2) 1.0851(3) 0.0604(16) Uani 1 1 d . . . . .
C35 C 1.3536(5) 0.5317(3) 0.6393(3) 0.0286(18) Uani 1 1 d . . . . .
C36 C 0.4266(5) 0.4499(3) 0.9539(4) 0.0332(19) Uani 1 1 d . . . . .
H36 H 0.4037 0.4815 0.9698 0.040 Uiso 1 1 calc R . . . .
F37 F 0.9390(4) 0.3381(3) 0.3397(3) 0.081(2) Uani 1 1 d . . . . .
C38 C 1.1269(5) 0.4033(3) 0.7351(4) 0.0348(19) Uani 1 1 d . . . . .
C39 C 0.5822(5) 0.5751(3) 0.7081(4) 0.0293(18) Uani 1 1 d . . . . .
H39 H 0.5315 0.5558 0.6955 0.035 Uiso 1 1 calc R . . . .
C40 C 0.6031(5) 0.2225(3) 0.7154(3) 0.0255(17) Uani 1 1 d . . . . .
F41 F 1.3105(4) 0.3254(2) 0.6688(3) 0.0704(19) Uani 1 1 d . . . . .
C42 C 0.4019(5) 0.4010(3) 0.9782(4) 0.0324(19) Uani 1 1 d . . . . .
F43 F 0.8412(4) 0.3172(3) 0.4041(3) 0.091(2) Uani 1 1 d . . . . .
C44 C 0.5212(5) 0.4060(3) 0.8825(4) 0.0273(17) Uani 1 1 d . . . . .
F46 F 0.9693(4) 0.2776(3) 0.4064(3) 0.0699(18) Uani 1 1 d . . . . .
F47 F 1.3723(4) 0.3825(3) 0.7682(3) 0.077(2) Uani 1 1 d . . . . .
C48 C 1.3978(5) 0.5791(3) 0.6112(4) 0.0287(18) Uani 1 1 d . . . . .
C49 C 1.0703(5) 0.3730(3) 0.4408(3) 0.0298(18) Uani 1 1 d . . . . .
C50 C 0.3986(6) 0.3828(4) 1.0871(4) 0.039(2) Uani 1 1 d . . . . .
F51 F 1.2681(4) 0.3322(3) 0.8023(3) 0.0692(18) Uani 1 1 d . . . . .
C52 C 1.2265(6) 0.3925(3) 0.7213(4) 0.036(2) Uani 1 1 d . . . . .
C54 C 0.5847(5) 0.4077(3) 0.8323(3) 0.0279(18) Uani 1 1 d . . . . .
C55 C 0.4845(5) 0.4524(3) 0.9066(4) 0.0338(19) Uani 1 1 d . . . . .
H55 H 0.4994 0.4857 0.8905 0.041 Uiso 1 1 calc R . . . .
C56 C 0.8831(5) 0.3078(3) 0.6146(4) 0.0335(19) Uani 1 1 d . . . . .
C57 C 0.4971(6) 0.3571(3) 0.9077(4) 0.040(2) Uani 1 1 d . . . . .
H57 H 0.5204 0.3254 0.8923 0.047 Uiso 1 1 calc R . . . .
C58 C 1.3566(6) 0.3763(3) 0.4579(4) 0.035(2) Uani 1 1 d . . . . .
C59 C 0.9629(5) 0.2921(3) 0.5906(4) 0.037(2) Uani 1 1 d . . . . .
H59 H 0.9994 0.2674 0.6112 0.044 Uiso 1 1 calc R . . . .
C60 C 1.2044(6) 0.4064(4) 0.4891(4) 0.040(2) Uani 1 1 d . . . . .
H60 H 1.2318 0.4281 0.5185 0.048 Uiso 1 1 calc R . . . .
C61 C 1.1137(5) 0.4030(3) 0.4857(4) 0.0348(19) Uani 1 1 d . . . . .
H61 H 1.0798 0.4211 0.5140 0.042 Uiso 1 1 calc R . . . .
F62 F 0.8402(4) 0.4224(3) 0.4089(3) 0.086(2) Uani 1 1 d . . . . .
C63 C 1.5840(5) 0.2732(4) 0.4656(4) 0.035(2) Uani 1 1 d . . . . .
C64 C 0.8184(5) 0.2699(3) 0.8499(4) 0.0265(17) Uani 1 1 d . . . . .
C66 C 0.2701(5) 0.3490(3) 1.0170(4) 0.036(2) Uani 1 1 d . . . . .
C67 C 1.3115(5) 0.5358(3) 0.6938(4) 0.0319(18) Uani 1 1 d . . . . .
H67 H 1.3109 0.5685 0.7140 0.038 Uiso 1 1 calc R . . . .
C68 C 1.2578(5) 0.3779(3) 0.4491(3) 0.0300(18) Uani 1 1 d . . . . .
C69 C 1.3159(5) 0.4373(3) 0.6376(4) 0.0330(19) Uani 1 1 d . . . . .
H69 H 1.3199 0.4041 0.6187 0.040 Uiso 1 1 calc R . . . .
C70 C 0.8320(6) 0.3460(4) 0.5838(4) 0.043(2) Uani 1 1 d . . . . .
H70 H 0.7780 0.3572 0.5999 0.051 Uiso 1 1 calc R . . . .
C71 C 0.9895(6) 0.3126(3) 0.5363(4) 0.040(2) Uani 1 1 d . . . . .
H71 H 1.0434 0.3009 0.5204 0.048 Uiso 1 1 calc R . . . .
C72 C 0.9381(5) 0.3502(3) 0.5043(4) 0.0335(19) Uani 1 1 d . . . . .
C74 C 0.2332(7) 0.3475(4) 0.9593(4) 0.050(3) Uani 1 1 d . . . . .
H74 H 0.2499 0.3730 0.9311 0.060 Uiso 1 1 calc R . . . .
C75 C 0.1816(6) 0.2726(4) 1.0429(4) 0.039(2) Uani 1 1 d . . . . .
H75 H 0.1647 0.2474 1.0715 0.047 Uiso 1 1 calc R . . . .
C76 C 0.5201(5) 0.1978(3) 0.6887(4) 0.0301(18) Uani 1 1 d . . . . .
C77 C 1.0785(6) 0.4412(4) 0.7016(4) 0.045(2) Uani 1 1 d . . . . .
H77 H 1.1078 0.4620 0.6733 0.054 Uiso 1 1 calc R . . . .
C78 C 1.2720(5) 0.4414(3) 0.6899(4) 0.0316(18) Uani 1 1 d . . . . .
C79 C 0.3391(5) 0.3948(3) 1.0319(3) 0.0304(18) Uani 1 1 d . . . . .
C80 C 1.2841(6) 0.3810(4) 0.7792(5) 0.049(3) Uani 1 1 d . . . . .
C81 C 0.9664(6) 0.3676(4) 0.4410(4) 0.044(2) Uani 1 1 d . . . . .
C82 C 1.2271(7) 0.3427(4) 0.6799(5) 0.054(3) Uani 1 1 d . . . . .
C83 C 1.1225(6) 0.3471(3) 0.3984(4) 0.036(2) Uani 1 1 d . . . . .
H83 H 1.0952 0.3279 0.3668 0.044 Uiso 1 1 calc R . . . .
C84 C 0.2816(6) 0.4457(4) 1.0434(4) 0.045(2) Uani 1 1 d . . . . .
C85 C 1.2152(5) 0.3500(3) 0.4036(4) 0.035(2) Uani 1 1 d . . . . .
H85 H 1.2496 0.3324 0.3752 0.043 Uiso 1 1 calc R . . . .
C86 C 0.1709(7) 0.3078(4) 0.9430(4) 0.048(2) Uani 1 1 d . . . . .
H86 H 0.1465 0.3068 0.9039 0.057 Uiso 1 1 calc R . . . .
C87 C 0.9874(6) 0.4487(4) 0.7096(5) 0.048(3) Uani 1 1 d . . . . .
H87 H 0.9564 0.4756 0.6886 0.058 Uiso 1 1 calc R . . . .
C88 C 0.3129(6) 0.2034(3) 0.4091(4) 0.0331(19) Uani 1 1 d . . . . .
C89 C 0.4395(6) 0.3548(3) 0.9548(4) 0.040(2) Uani 1 1 d . . . . .
H89 H 0.4255 0.3216 0.9714 0.048 Uiso 1 1 calc R . . . .
F90 F 0.3460(9) 0.0565(3) 0.5642(5) 0.142(5) Uani 1 1 d . . . . .
C91 C 0.3669(7) 0.1576(4) 0.6299(4) 0.052(3) Uani 1 1 d . . . . .
C92 C 1.6454(6) 0.2297(3) 0.4847(4) 0.0330(19) Uani 1 1 d . . . . .
C93 C 1.3553(5) 0.4820(3) 0.6113(4) 0.0330(19) Uani 1 1 d . . . . .
H93 H 1.3833 0.4784 0.5745 0.040 Uiso 1 1 calc R . . . .
C94 C 0.9278(6) 0.4228(5) 0.4217(5) 0.058(3) Uani 1 1 d . . . . .
C95 C 0.2824(7) 0.1398(4) 0.5912(5) 0.059(3) Uani 1 1 d . . . . .
C96 C 0.9295(7) 0.3248(6) 0.3967(5) 0.063(3) Uani 1 1 d . . . . .
C97 C 0.2431(6) 0.3123(4) 1.0585(4) 0.039(2) Uani 1 1 d . . . . .
H97 H 0.2663 0.3140 1.0979 0.046 Uiso 1 1 calc R . . . .
C98 C 0.9425(5) 0.4154(3) 0.7495(4) 0.038(2) Uani 1 1 d . . . . .
C99 C 0.9899(6) 0.3760(4) 0.7811(5) 0.054(3) Uani 1 1 d . . . . .
H99 H 0.9597 0.3525 0.8061 0.065 Uiso 1 1 calc R . . . .
C100 C 0.8588(6) 0.3678(4) 0.5306(4) 0.048(2) Uani 1 1 d . . . . .
H100 H 0.8241 0.3944 0.5117 0.057 Uiso 1 1 calc R . . . .
F101 F 0.2017(8) 0.0639(3) 0.5602(6) 0.184(6) Uani 1 1 d . . . . .
F102 F 0.1911(5) 0.2141(6) 0.6135(4) 0.130(4) Uani 1 1 d . . . . .
C104 C 1.2701(6) 0.4915(4) 0.7184(4) 0.039(2) Uani 1 1 d . . . . .
H104 H 1.2405 0.4952 0.7546 0.047 Uiso 1 1 calc R . . . .
F105 F 0.2721(7) 0.0597(5) 0.6454(5) 0.163(5) Uani 1 1 d . . . . .
C106 C 1.0801(6) 0.3713(4) 0.7756(4) 0.050(3) Uani 1 1 d . . . . .
H106 H 1.1115 0.3464 0.7994 0.060 Uiso 1 1 calc R . . . .
C107 C 0.2948(6) 0.1604(4) 0.5252(4) 0.044(2) Uani 1 1 d . . . . .
C108 C 0.3802(12) 0.1677(8) 0.4988(8) 0.061(6) Uani 0.595(15) 1 d . . P A 1
H108 H 0.4314 0.1567 0.5206 0.073 Uiso 0.595(15) 1 calc R . P A 1
C109 C 0.2000(9) 0.1563(9) 0.6152(7) 0.103(6) Uani 1 1 d . . . . .
C110 C 0.4540(9) 0.2304(6) 0.6648(7) 0.040(4) Uani 0.617(16) 1 d . . P B 1
H110 H 0.4559 0.2674 0.6706 0.048 Uiso 0.617(16) 1 calc R . P B 1
C113 C 0.3849(11) 0.2071(6) 0.6322(8) 0.051(5) Uani 0.617(16) 1 d . . P B 1
H113 H 0.3477 0.2299 0.6096 0.061 Uiso 0.617(16) 1 calc R . P B 1
F114 F 0.1892(9) 0.1499(6) 0.6752(5) 0.201(7) Uani 1 1 d . . . . .
C117 C 0.2705(11) 0.0831(6) 0.5912(9) 0.105(6) Uani 1 1 d . . . . .
F142 F 0.1249(6) 0.1438(8) 0.5884(7) 0.268(10) Uani 1 1 d . . . . .
O1 O 1.5467(4) 0.2841(2) 0.2798(3) 0.0405(14) Uani 1 1 d . . . . .
H1A H 1.5065 0.2705 0.2564 0.061 Uiso 1 1 d GR . . . .
H1B H 1.5819 0.2594 0.2926 0.061 Uiso 1 1 d GR . . . .
O2 O 0.7989(4) 0.3799(3) 0.7688(3) 0.0462(16) Uani 1 1 d . . . . .
N28 N 0.6281(4) 0.3774(2) 0.6773(3) 0.0265(14) Uani 1 1 d . . . . .
O0AA O 0.6053(4) 0.4536(2) 0.8114(2) 0.0363(14) Uani 1 1 d . . . . .
O5 O 0.8084(4) 0.4663(3) 0.7453(3) 0.0471(16) Uani 1 1 d . . . . .
N6 N 1.5708(4) 0.3984(2) 0.5870(3) 0.0262(14) Uani 1 1 d . . . . .
F7 F 0.9675(4) 0.4416(3) 0.3737(3) 0.088(2) Uani 1 1 d . . . . .
C8 C 0.5964(5) 0.4429(3) 0.6168(3) 0.0311(18) Uani 1 1 d . . . . .
H8 H 0.5908 0.4775 0.6011 0.037 Uiso 1 1 calc R . . . .
C0AA C 0.5908(5) 0.3589(3) 0.6269(3) 0.0244(16) Uani 1 1 d . . . . .
H0AA H 0.5795 0.3226 0.6195 0.029 Uiso 1 1 calc R . . . .
N10 N 0.6304(4) 0.4320(2) 0.6711(3) 0.0283(15) Uani 1 1 d . . . . .
C1AA C 0.8428(5) 0.4202(3) 0.7548(4) 0.035(2) Uani 1 1 d . . . . .
C12 C 0.8486(5) 0.2803(3) 0.6699(3) 0.0296(18) Uani 1 1 d . . . . .
C13 C 0.3913(12) 0.1914(7) 0.4397(7) 0.050(5) Uani 0.595(15) 1 d . . P A 1
H13 H 0.4475 0.1980 0.4238 0.060 Uiso 0.595(15) 1 calc R . P A 1
C14 C 0.2264(12) 0.1921(9) 0.4309(7) 0.047(5) Uani 0.595(15) 1 d . . P A 1
H14 H 0.1753 0.1988 0.4069 0.056 Uiso 0.595(15) 1 calc R . P A 1
C17 C 0.4361(15) 0.1221(8) 0.6511(10) 0.074(7) Uani 0.617(16) 1 d . . P B 1
H17 H 0.4314 0.0853 0.6442 0.088 Uiso 0.617(16) 1 calc R . P B 1
C19 C 0.5097(11) 0.1428(6) 0.6820(9) 0.050(5) Uani 0.617(16) 1 d . . P B 1
H19 H 0.5529 0.1196 0.6986 0.060 Uiso 0.617(16) 1 calc R . P B 1
C1 C 0.2588(13) 0.1373(10) 0.4761(9) 0.028(5) Uani 0.405(15) 1 d . . P A 2
H1 H 0.2283 0.1049 0.4801 0.034 Uiso 0.405(15) 1 calc R . P A 2
C2 C 0.3580(16) 0.1974(8) 0.6787(10) 0.033(5) Uani 0.383(16) 1 d . U P B 2
H2 H 0.3018 0.2092 0.6905 0.040 Uiso 0.383(16) 1 calc R . P B 2
C3 C 0.5247(14) 0.1587(8) 0.6432(11) 0.030(4) Uani 0.383(16) 1 d . U P B 2
H3 H 0.5800 0.1452 0.6317 0.036 Uiso 0.383(16) 1 calc R . P B 2
C4 C 0.2653(15) 0.1600(11) 0.4191(10) 0.039(6) Uani 0.405(15) 1 d . . P A 2
H4 H 0.2347 0.1438 0.3866 0.046 Uiso 0.405(15) 1 calc R . P A 2
C5 C 0.3453(14) 0.2099(9) 0.5185(9) 0.033(6) Uani 0.405(15) 1 d . . P A 2
H5 H 0.3712 0.2277 0.5517 0.040 Uiso 0.405(15) 1 calc R . P A 2
C400 C 0.2184(12) 0.1710(8) 0.4883(7) 0.050(5) Uani 0.595(15) 1 d . . P A 1
H400 H 0.1616 0.1636 0.5026 0.060 Uiso 0.595(15) 1 calc R . P A 1
C6 C 0.3529(15) 0.2297(9) 0.4589(9) 0.038(6) Uani 0.405(15) 1 d . . P A 2
H6 H 0.3855 0.2610 0.4526 0.046 Uiso 0.405(15) 1 calc R . P A 2
C7 C 0.4369(15) 0.2170(8) 0.7066(11) 0.032(5) Uani 0.383(16) 1 d . U P B 2
H7 H 0.4338 0.2427 0.7370 0.038 Uiso 0.383(16) 1 calc R . P B 2
C9 C 0.4443(14) 0.1402(9) 0.6151(11) 0.029(4) Uani 0.383(16) 1 d . U P B 2
H9 H 0.4475 0.1145 0.5847 0.034 Uiso 0.383(16) 1 calc R . P B 2
O11 O 1.7119(18) 0.3074(11) 0.2925(14) 0.153(16) Uani 0.48(3) 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
Co1 0.0242(6) 0.0243(6) 0.0165(6) -0.0005(5) 0.0011(5) 0.0029(5)
Co2 0.0276(6) 0.0138(6) 0.0222(6) 0.0001(5) 0.0015(5) -0.0022(5)
Co3 0.0257(6) 0.0218(6) 0.0239(6) -0.0029(5) -0.0005(5) 0.0014(5)
Co4 0.0271(6) 0.0154(6) 0.0257(7) 0.0023(5) 0.0002(5) 0.0019(5)
Co5 0.0244(6) 0.0179(6) 0.0220(6) -0.0004(5) 0.0014(5) -0.0003(5)
F2 0.054(3) 0.035(3) 0.051(3) 0.006(2) -0.002(3) -0.005(2)
O1AA 0.031(3) 0.040(3) 0.031(3) -0.005(3) 0.002(2) -0.006(2)
O4 0.029(3) 0.036(3) 0.025(3) 0.000(2) -0.006(2) 0.001(2)
O3AA 0.040(3) 0.032(3) 0.024(3) -0.008(2) 0.011(2) -0.001(2)
O6 0.050(4) 0.057(4) 0.035(3) -0.006(3) 0.021(3) 0.015(3)
O8 0.032(3) 0.020(3) 0.040(3) 0.000(2) -0.006(2) -0.004(2)
O10 0.041(3) 0.034(3) 0.029(3) 0.007(3) -0.015(3) -0.011(3)
F12 0.050(3) 0.040(3) 0.050(3) -0.006(2) -0.010(3) -0.018(2)
O13 0.050(4) 0.041(4) 0.031(3) 0.006(3) 0.004(3) -0.015(3)
O14 0.047(3) 0.036(3) 0.027(3) -0.010(3) -0.009(3) 0.016(3)
F15 0.049(3) 0.062(4) 0.067(4) 0.005(3) 0.000(3) 0.012(3)
F16 0.067(4) 0.083(4) 0.029(3) -0.007(3) 0.013(3) -0.019(3)
F17 0.055(3) 0.038(3) 0.065(4) -0.019(3) 0.014(3) -0.007(2)
O18 0.045(3) 0.035(3) 0.034(3) -0.003(3) -0.006(3) 0.011(3)
F19 0.081(4) 0.084(5) 0.040(3) 0.008(3) -0.001(3) -0.015(4)
N20 0.030(3) 0.025(4) 0.032(4) 0.002(3) -0.002(3) -0.004(3)
F21 0.055(4) 0.054(4) 0.107(6) 0.031(4) 0.016(4) 0.019(3)
O22 0.025(3) 0.065(4) 0.040(4) -0.009(3) -0.004(3) 0.010(3)
F23 0.101(5) 0.032(3) 0.096(5) 0.012(3) 0.034(4) -0.010(3)
N25 0.033(3) 0.019(3) 0.023(3) 0.002(3) -0.009(3) -0.005(3)
C26 0.033(4) 0.013(4) 0.039(5) 0.001(3) 0.006(4) 0.001(3)
N27 0.023(3) 0.019(3) 0.028(3) -0.004(3) -0.005(3) 0.002(2)
O28 0.037(3) 0.020(3) 0.086(5) -0.011(3) -0.019(3) 0.004(2)
O29 0.037(3) 0.036(3) 0.041(3) 0.013(3) 0.015(3) 0.002(3)
F30 0.072(4) 0.049(3) 0.053(4) -0.006(3) 0.006(3) -0.021(3)
O31 0.046(4) 0.054(4) 0.034(3) -0.005(3) 0.020(3) 0.003(3)
F33 0.054(3) 0.064(4) 0.065(4) -0.011(3) 0.033(3) -0.004(3)
C35 0.022(4) 0.043(5) 0.021(4) 0.002(4) -0.001(3) -0.006(3)
C36 0.037(4) 0.028(5) 0.035(5) -0.002(4) 0.009(4) -0.005(3)
F37 0.070(4) 0.138(6) 0.035(3) 0.002(4) -0.008(3) -0.025(4)
C38 0.031(4) 0.034(5) 0.039(5) 0.003(4) -0.001(4) 0.001(4)
C39 0.039(4) 0.014(4) 0.034(5) 0.002(3) -0.013(4) -0.008(3)
C40 0.028(4) 0.026(4) 0.022(4) 0.010(3) -0.002(3) -0.003(3)
F41 0.066(4) 0.039(3) 0.108(5) 0.013(3) 0.027(4) 0.018(3)
C42 0.036(4) 0.032(5) 0.030(4) -0.003(4) 0.007(4) -0.005(4)
F43 0.052(4) 0.136(7) 0.083(5) 0.002(5) -0.006(3) -0.049(4)
C44 0.033(4) 0.018(4) 0.031(4) -0.001(3) 0.005(3) -0.004(3)
F46 0.077(4) 0.069(4) 0.063(4) 0.001(3) -0.005(3) -0.029(4)
F47 0.031(3) 0.113(5) 0.086(5) 0.048(4) -0.003(3) 0.002(3)
C48 0.019(3) 0.038(5) 0.029(4) -0.004(4) 0.000(3) -0.003(3)
C49 0.031(4) 0.041(5) 0.018(4) 0.010(4) 0.001(3) 0.005(4)
C50 0.040(5) 0.043(5) 0.033(5) -0.002(4) 0.001(4) -0.011(4)
F51 0.058(3) 0.072(4) 0.078(4) 0.046(4) -0.001(3) 0.011(3)
C52 0.035(4) 0.036(5) 0.036(5) 0.011(4) 0.001(4) 0.004(4)
C54 0.031(4) 0.036(5) 0.018(4) -0.009(4) 0.004(3) 0.002(3)
C55 0.034(4) 0.023(4) 0.045(5) 0.004(4) 0.010(4) -0.005(3)
C56 0.034(4) 0.020(4) 0.046(5) 0.005(4) 0.010(4) 0.002(3)
C57 0.051(5) 0.028(5) 0.041(5) -0.003(4) 0.019(4) 0.002(4)
C58 0.049(5) 0.027(5) 0.029(5) 0.006(4) 0.017(4) 0.006(4)
C59 0.030(4) 0.040(5) 0.042(5) 0.012(4) 0.003(4) 0.008(4)
C60 0.036(5) 0.047(6) 0.036(5) -0.006(4) 0.002(4) -0.002(4)
C61 0.028(4) 0.045(5) 0.031(5) 0.000(4) 0.006(4) 0.004(4)
F62 0.040(3) 0.124(6) 0.094(5) 0.058(5) -0.003(3) 0.020(4)
C63 0.035(4) 0.043(5) 0.028(5) 0.003(4) 0.002(4) 0.000(4)
C64 0.029(4) 0.017(4) 0.033(4) 0.002(3) -0.002(4) -0.001(3)
C66 0.032(4) 0.040(5) 0.037(5) -0.006(4) 0.007(4) -0.014(4)
C67 0.030(4) 0.034(5) 0.032(4) -0.005(4) -0.001(4) -0.002(3)
C68 0.029(4) 0.041(5) 0.021(4) 0.000(4) 0.002(3) 0.005(3)
C69 0.032(4) 0.023(4) 0.044(5) -0.009(4) -0.002(4) -0.001(3)
C70 0.031(4) 0.041(5) 0.057(6) 0.013(5) 0.008(4) 0.013(4)
C71 0.034(4) 0.037(5) 0.050(6) 0.009(4) 0.018(4) 0.004(4)
C72 0.031(4) 0.035(5) 0.034(5) 0.009(4) 0.002(4) -0.006(3)
C74 0.060(6) 0.055(6) 0.036(5) 0.017(5) -0.011(5) -0.030(5)
C75 0.054(5) 0.042(5) 0.021(4) 0.010(4) 0.001(4) -0.020(4)
C76 0.032(4) 0.026(4) 0.032(5) 0.002(4) -0.004(4) -0.005(3)
C77 0.029(4) 0.051(6) 0.056(6) 0.026(5) 0.007(4) 0.000(4)
C78 0.031(4) 0.035(5) 0.030(4) 0.002(4) 0.010(4) -0.003(3)
C79 0.036(4) 0.036(5) 0.020(4) -0.006(3) 0.010(3) -0.013(4)
C80 0.034(5) 0.064(7) 0.049(6) 0.030(6) -0.011(4) 0.002(4)
C81 0.033(5) 0.049(6) 0.050(6) 0.012(5) 0.007(4) 0.003(4)
C82 0.050(6) 0.051(6) 0.061(7) 0.015(5) 0.016(5) 0.002(5)
C83 0.047(5) 0.039(5) 0.023(4) -0.003(4) -0.006(4) -0.009(4)
C84 0.046(5) 0.052(6) 0.038(5) -0.002(5) 0.017(5) -0.010(4)
C85 0.036(4) 0.046(5) 0.025(4) -0.005(4) 0.010(4) 0.004(4)
C86 0.064(6) 0.049(6) 0.029(5) 0.008(4) -0.024(5) -0.023(5)
C87 0.038(5) 0.044(6) 0.062(6) 0.031(5) 0.008(5) 0.004(4)
C88 0.045(5) 0.032(5) 0.022(4) 0.009(4) -0.010(4) -0.013(4)
C89 0.057(5) 0.018(4) 0.046(5) 0.005(4) 0.020(5) -0.007(4)
F90 0.239(12) 0.043(4) 0.135(8) -0.011(5) -0.134(9) -0.009(6)
C91 0.064(7) 0.046(6) 0.043(6) 0.021(5) -0.018(5) -0.019(5)
C92 0.042(5) 0.022(4) 0.035(5) -0.002(4) 0.005(4) 0.010(3)
C93 0.033(4) 0.038(5) 0.029(4) -0.005(4) 0.009(4) 0.004(4)
C94 0.033(5) 0.081(8) 0.060(7) 0.030(7) -0.003(5) 0.010(5)
C95 0.060(7) 0.064(7) 0.051(6) 0.011(5) -0.014(5) -0.030(5)
C96 0.037(5) 0.103(10) 0.050(7) 0.016(7) 0.000(5) -0.028(6)
C97 0.045(5) 0.051(6) 0.019(4) 0.008(4) -0.005(4) -0.027(4)
C98 0.028(4) 0.037(5) 0.050(6) -0.003(4) 0.007(4) -0.003(4)
C99 0.037(5) 0.055(6) 0.071(7) 0.033(6) 0.016(5) -0.005(4)
C100 0.038(5) 0.049(6) 0.056(6) 0.023(5) 0.011(5) 0.015(4)
F101 0.193(10) 0.080(6) 0.269(14) 0.041(7) -0.171(10) -0.083(7)
F102 0.062(5) 0.244(13) 0.083(6) -0.038(8) -0.011(4) 0.050(7)
C104 0.042(5) 0.043(5) 0.032(5) -0.007(4) 0.012(4) -0.003(4)
F105 0.139(8) 0.184(10) 0.165(9) 0.143(9) -0.043(7) -0.081(7)
C106 0.038(5) 0.063(7) 0.048(6) 0.028(5) 0.005(4) -0.002(4)
C107 0.055(6) 0.036(5) 0.039(5) 0.012(4) -0.011(5) -0.014(4)
C108 0.064(12) 0.079(15) 0.038(10) 0.023(10) -0.039(9) -0.003(10)
C109 0.043(7) 0.197(19) 0.068(9) -0.010(11) -0.006(7) -0.062(10)
C110 0.039(8) 0.036(9) 0.043(10) 0.005(7) -0.015(7) -0.007(6)
C113 0.058(10) 0.038(10) 0.053(12) 0.012(8) -0.031(9) -0.007(7)
F114 0.242(14) 0.271(15) 0.095(7) -0.028(9) 0.085(9) -0.156(12)
C117 0.105(11) 0.066(10) 0.141(15) 0.057(10) -0.074(11) -0.054(8)
F142 0.051(5) 0.44(2) 0.308(18) -0.240(18) 0.009(8) -0.071(9)
O1 0.042(3) 0.046(4) 0.034(3) -0.011(3) -0.005(3) 0.013(3)
O2 0.037(3) 0.046(4) 0.056(4) 0.002(3) -0.002(3) -0.015(3)
N28 0.039(4) 0.015(3) 0.026(3) 0.002(3) 0.001(3) 0.001(3)
O0AA 0.052(3) 0.025(3) 0.033(3) 0.003(3) 0.015(3) -0.009(3)
O5 0.026(3) 0.046(4) 0.069(5) 0.009(3) 0.004(3) -0.001(3)
N6 0.036(4) 0.018(3) 0.025(3) -0.001(3) 0.010(3) 0.006(3)
F7 0.061(4) 0.112(6) 0.094(5) 0.075(5) 0.026(4) 0.023(4)
C8 0.046(5) 0.027(4) 0.019(4) -0.008(3) -0.010(4) -0.003(4)
C0AA 0.036(4) 0.019(4) 0.017(4) 0.001(3) -0.009(3) -0.006(3)
N10 0.041(4) 0.014(3) 0.030(4) 0.003(3) 0.000(3) 0.001(3)
C1AA 0.033(4) 0.028(5) 0.043(5) -0.007(4) -0.001(4) -0.013(4)
C12 0.039(4) 0.033(5) 0.017(4) -0.013(3) -0.005(3) 0.001(4)
C13 0.068(11) 0.040(10) 0.041(10) 0.017(8) -0.037(9) -0.009(9)
C14 0.036(9) 0.084(15) 0.021(8) 0.011(9) -0.002(7) -0.005(9)
C17 0.105(16) 0.048(12) 0.068(15) -0.002(11) -0.006(12) -0.053(12)
C19 0.058(10) 0.031(9) 0.059(13) -0.004(8) -0.021(9) -0.009(7)
C1 0.024(10) 0.038(13) 0.021(11) -0.008(9) -0.015(8) -0.001(9)
C2 0.053(10) 0.022(8) 0.023(10) 0.001(7) -0.008(8) -0.007(7)
C3 0.035(8) 0.022(9) 0.034(10) 0.011(8) 0.015(8) -0.004(7)
C4 0.032(12) 0.066(18) 0.018(11) 0.004(11) -0.010(9) 0.000(12)
C5 0.044(12) 0.031(13) 0.024(11) -0.003(9) -0.009(9) -0.021(10)
C400 0.045(10) 0.073(14) 0.031(9) 0.002(9) -0.020(8) -0.016(10)
C6 0.057(14) 0.026(13) 0.030(12) 0.017(10) -0.005(10) 0.007(10)
C7 0.054(10) 0.019(8) 0.023(10) -0.001(7) -0.008(8) -0.010(7)
C9 0.034(9) 0.022(9) 0.031(10) 0.011(8) 0.015(8) -0.005(7)
O11 0.13(2) 0.14(3) 0.19(3) -0.05(2) 0.02(2) 0.012(18)
_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
Co1 O13 1.944(5) 3_866 ?
Co1 O14 1.936(5) . ?
Co1 O22 1.976(5) . ?
Co1 N6 2.051(6) . ?
Co2 N25 2.004(6) . ?
Co2 O0AA 1.928(5) . ?
Co2 O5 1.941(6) . ?
Co2 N10 2.019(6) . ?
Co3 O1AA 2.100(5) 3_866 ?
Co3 O6 2.090(5) . ?
Co3 O10 2.165(5) . ?
Co3 O18 1.986(6) . ?
Co3 N20 2.103(6) . ?
Co3 O1 2.111(5) . ?
Co4 O4 2.047(5) . ?
Co4 O10 2.379(5) 4_566 ?
Co4 N27 2.027(6) . ?
Co4 O28 1.971(6) . ?
Co4 O29 2.057(5) . ?
Co4 O31 2.368(6) . ?
Co5 O4 2.250(5) . ?
Co5 O3AA 2.001(5) . ?
Co5 O8 2.053(5) . ?
Co5 O31 2.127(6) . ?
Co5 O2 2.071(6) . ?
Co5 N28 2.129(6) . ?
F2 C50 1.330(10) . ?
O1AA Co3 2.100(5) 3_866 ?
O1AA C48 1.243(9) . ?
O4 C64 1.272(9) . ?
O3AA C54 1.248(9) . ?
O6 C58 1.244(9) . ?
O8 C40 1.251(9) . ?
O10 Co4 2.379(5) 4_665 ?
O10 C64 1.266(9) 4_665 ?
F12 C50 1.339(9) . ?
O13 Co1 1.944(5) 3_866 ?
O13 C48 1.281(9) . ?
O14 C63 1.278(10) . ?
F15 C84 1.315(11) . ?
F16 C50 1.346(10) . ?
F17 C84 1.337(10) . ?
O18 C63 1.284(10) . ?
F19 C80 1.329(12) . ?
N20 N27 1.400(8) 4_665 ?
N20 C39 1.307(10) 3_766 ?
F21 C94 1.349(14) . ?
O22 C58 1.278(10) . ?
F23 C82 1.340(11) . ?
N25 C26 1.350(9) . ?
N25 C39 1.359(9) . ?
C26 H26 0.9300 . ?
C26 N27 1.321(9) 2_656 ?
N27 N20 1.400(8) 4_566 ?
N27 C26 1.321(9) 2_646 ?
O28 C40 1.258(9) . ?
O29 C12 1.263(9) . ?
F30 C82 1.322(12) . ?
O31 C12 1.260(9) . ?
F33 C84 1.335(10) . ?
C35 C48 1.495(11) . ?
C35 C67 1.377(11) . ?
C35 C93 1.384(11) . ?
C36 H36 0.9300 . ?
C36 C42 1.383(11) . ?
C36 C55 1.376(11) . ?
F37 C96 1.316(12) . ?
C38 C52 1.544(11) . ?
C38 C77 1.388(12) . ?
C38 C106 1.399(12) . ?
C39 N20 1.307(10) 3_766 ?
C39 H39 0.9300 . ?
C40 C76 1.486(10) . ?
F41 C82 1.341(11) . ?
C42 C79 1.539(10) . ?
C42 C89 1.386(11) . ?
F43 C96 1.341(11) . ?
C44 C54 1.480(10) . ?
C44 C55 1.390(11) . ?
C44 C57 1.387(11) . ?
F46 C96 1.330(14) . ?
F47 C80 1.340(10) . ?
C49 C61 1.389(12) . ?
C49 C81 1.550(11) . ?
C49 C83 1.393(11) . ?
C50 C79 1.518(12) . ?
F51 C80 1.341(11) . ?
C52 C78 1.564(11) . ?
C52 C80 1.550(12) . ?
C52 C82 1.540(14) . ?
C54 O0AA 1.272(9) . ?
C55 H55 0.9300 . ?
C56 C59 1.371(11) . ?
C56 C70 1.384(11) . ?
C56 C12 1.505(11) . ?
C57 H57 0.9300 . ?
C57 C89 1.369(11) . ?
C58 C68 1.478(11) . ?
C59 H59 0.9300 . ?
C59 C71 1.375(12) . ?
C60 H60 0.9300 . ?
C60 C61 1.351(11) . ?
C60 C68 1.398(11) . ?
C61 H61 0.9300 . ?
F62 C94 1.325(11) . ?
C63 C92 1.470(11) . ?
C64 O10 1.266(9) 4_566 ?
C64 C88 1.474(11) 4_666 ?
C66 C74 1.377(12) . ?
C66 C79 1.561(10) . ?
C66 C97 1.363(11) . ?
C67 H67 0.9300 . ?
C67 C104 1.380(12) . ?
C68 C85 1.367(12) . ?
C69 H69 0.9300 . ?
C69 C78 1.351(11) . ?
C69 C93 1.390(11) . ?
C70 H70 0.9300 . ?
C70 C100 1.367(12) . ?
C71 H71 0.9300 . ?
C71 C72 1.390(12) . ?
C72 C81 1.536(12) . ?
C72 C100 1.400(12) . ?
C74 H74 0.9300 . ?
C74 C86 1.394(12) . ?
C75 H75 0.9300 . ?
C75 C92 1.382(12) 4_466 ?
C75 C97 1.383(11) . ?
C76 C110 1.369(16) . ?
C76 C19 1.386(17) . ?
C76 C3 1.40(2) . ?
C76 C7 1.39(2) . ?
C77 H77 0.9300 . ?
C77 C87 1.384(12) . ?
C78 C104 1.397(12) . ?
C79 C84 1.553(13) . ?
C81 C94 1.544(14) . ?
C81 C96 1.537(15) . ?
C83 H83 0.9300 . ?
C83 C85 1.381(11) . ?
C85 H85 0.9300 . ?
C86 H86 0.9300 . ?
C86 C92 1.374(11) 4_466 ?
C87 H87 0.9300 . ?
C87 C98 1.394(12) . ?
C88 C64 1.474(11) 4_565 ?
C88 C13 1.364(17) . ?
C88 C14 1.415(18) . ?
C88 C4 1.31(3) . ?
C88 C6 1.40(2) . ?
C89 H89 0.9300 . ?
F90 C117 1.45(2) . ?
C91 C95 1.565(13) . ?
C91 C113 1.261(17) . ?
C91 C17 1.42(2) . ?
C91 C2 1.47(2) . ?
C91 C9 1.28(2) . ?
C92 C75 1.382(12) 4_765 ?
C92 C86 1.374(11) 4_765 ?
C93 H93 0.9300 . ?
C94 F7 1.317(11) . ?
C95 C107 1.565(13) . ?
C95 C109 1.409(19) . ?
C95 C117 1.422(17) . ?
C97 H97 0.9300 . ?
C98 C99 1.385(13) . ?
C98 C1AA 1.495(11) . ?
C99 H99 0.9300 . ?
C99 C106 1.354(12) . ?
C100 H100 0.9300 . ?
F101 C117 1.306(14) . ?
F102 C109 1.44(2) . ?
C104 H104 0.9300 . ?
F105 C117 1.332(17) . ?
C106 H106 0.9300 . ?
C107 C108 1.42(2) . ?
C107 C1 1.33(2) . ?
C107 C5 1.45(2) . ?
C107 C400 1.405(18) . ?
C108 H108 0.9300 . ?
C108 C13 1.45(2) . ?
C109 F114 1.353(17) . ?
C109 F142 1.287(14) . ?
C110 H110 0.9300 . ?
C110 C113 1.367(19) . ?
C113 H113 0.9300 . ?
O1 H1A 0.8503 . ?
O1 H1B 0.8504 . ?
O2 C1AA 1.239(10) . ?
N28 C0AA 1.315(9) . ?
N28 N10 1.366(8) . ?
O5 C1AA 1.272(10) . ?
N6 C8 1.338(9) 1_655 ?
N6 C0AA 1.348(9) 1_655 ?
C8 N6 1.338(9) 1_455 ?
C8 H8 0.9300 . ?
C8 N10 1.319(10) . ?
C0AA N6 1.348(9) 1_455 ?
C0AA H0AA 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C400 1.38(2) . ?
C17 H17 0.9300 . ?
C17 C19 1.37(2) . ?
C19 H19 0.9300 . ?
C1 H1 0.9300 . ?
C1 C4 1.39(3) . ?
C2 H2 0.9300 . ?
C2 C7 1.40(3) . ?
C3 H3 0.9300 . ?
C3 C9 1.41(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.42(3) . ?
C400 H400 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C9 H9 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Co1 O22 110.9(3) 3_866 . ?
O13 Co1 N6 109.0(2) 3_866 . ?
O14 Co1 O13 115.7(3) . 3_866 ?
O14 Co1 O22 121.0(3) . . ?
O14 Co1 N6 92.8(2) . . ?
O22 Co1 N6 104.4(2) . . ?
N25 Co2 N10 109.4(2) . . ?
O0AA Co2 N25 105.1(2) . . ?
O0AA Co2 O5 123.5(3) . . ?
O0AA Co2 N10 107.6(2) . . ?
O5 Co2 N25 103.2(3) . . ?
O5 Co2 N10 107.4(3) . . ?
O1AA Co3 O10 171.4(2) 3_866 . ?
O1AA Co3 N20 86.2(2) 3_866 . ?
O1AA Co3 O1 90.7(2) 3_866 . ?
O6 Co3 O1AA 97.1(2) . 3_866 ?
O6 Co3 O10 89.7(2) . . ?
O6 Co3 N20 85.1(3) . . ?
O6 Co3 O1 170.9(3) . . ?
O18 Co3 O1AA 92.5(2) . 3_866 ?
O18 Co3 O6 94.0(2) . . ?
O18 Co3 O10 92.3(2) . . ?
O18 Co3 N20 178.4(2) . . ?
O18 Co3 O1 90.5(2) . . ?
N20 Co3 O10 89.1(2) . . ?
N20 Co3 O1 90.6(2) . . ?
O1 Co3 O10 82.1(2) . . ?
O4 Co4 O10 58.18(19) . 4_566 ?
O4 Co4 O29 114.7(2) . . ?
O4 Co4 O31 81.4(2) . . ?
N27 Co4 O4 122.7(2) . . ?
N27 Co4 O10 84.9(2) . 4_566 ?
N27 Co4 O29 104.7(2) . . ?
N27 Co4 O31 155.8(2) . . ?
O28 Co4 O4 98.1(2) . . ?
O28 Co4 O10 147.0(3) . 4_566 ?
O28 Co4 N27 91.2(2) . . ?
O28 Co4 O29 124.6(3) . . ?
O28 Co4 O31 85.6(2) . . ?
O29 Co4 O10 87.9(2) . 4_566 ?
O29 Co4 O31 59.0(2) . . ?
O31 Co4 O10 110.3(2) . 4_566 ?
O3AA Co5 O4 92.4(2) . . ?
O3AA Co5 O8 94.1(2) . . ?
O3AA Co5 O31 174.9(2) . . ?
O3AA Co5 O2 94.2(2) . . ?
O3AA Co5 N28 95.3(2) . . ?
O8 Co5 O4 84.2(2) . . ?
O8 Co5 O31 84.3(2) . . ?
O8 Co5 O2 167.8(2) . . ?
O8 Co5 N28 88.7(2) . . ?
O31 Co5 O4 82.6(2) . . ?
O31 Co5 N28 89.5(2) . . ?
O2 Co5 O4 86.5(2) . . ?
O2 Co5 O31 86.6(3) . . ?
O2 Co5 N28 99.5(2) . . ?
N28 Co5 O4 169.8(2) . . ?
C48 O1AA Co3 137.3(5) . 3_866 ?
Co4 O4 Co5 98.0(2) . . ?
C64 O4 Co4 99.6(5) . . ?
C64 O4 Co5 136.9(5) . . ?
C54 O3AA Co5 141.9(5) . . ?
C58 O6 Co3 173.4(6) . . ?
C40 O8 Co5 136.3(5) . . ?
Co3 O10 Co4 110.5(2) . 4_665 ?
C64 O10 Co3 152.8(5) 4_665 . ?
C64 O10 Co4 84.4(4) 4_665 4_665 ?
C48 O13 Co1 132.7(5) . 3_866 ?
C63 O14 Co1 134.0(5) . . ?
C63 O18 Co3 139.9(6) . . ?
N27 N20 Co3 121.9(4) 4_665 . ?
C39 N20 Co3 128.0(5) 3_766 . ?
C39 N20 N27 105.4(6) 3_766 4_665 ?
C58 O22 Co1 104.8(5) . . ?
C26 N25 Co2 131.1(5) . . ?
C26 N25 C39 102.4(6) . . ?
C39 N25 Co2 126.5(5) . . ?
N25 C26 H26 123.7 . . ?
N27 C26 N25 112.7(7) 2_656 . ?
N27 C26 H26 123.7 2_656 . ?
N20 N27 Co4 121.7(4) 4_566 . ?
C26 N27 Co4 130.7(5) 2_646 . ?
C26 N27 N20 106.0(6) 2_646 4_566 ?
C40 O28 Co4 126.1(5) . . ?
C12 O29 Co4 96.8(5) . . ?
Co5 O31 Co4 92.2(2) . . ?
C12 O31 Co4 82.8(5) . . ?
C12 O31 Co5 147.5(6) . . ?
C67 C35 C48 121.5(7) . . ?
C67 C35 C93 118.2(7) . . ?
C93 C35 C48 120.3(7) . . ?
C42 C36 H36 119.5 . . ?
C55 C36 H36 119.5 . . ?
C55 C36 C42 120.9(8) . . ?
C77 C38 C52 119.9(7) . . ?
C77 C38 C106 117.9(8) . . ?
C106 C38 C52 121.7(7) . . ?
N20 C39 N25 113.5(6) 3_766 . ?
N20 C39 H39 123.2 3_766 . ?
N25 C39 H39 123.2 . . ?
O8 C40 O28 125.6(7) . . ?
O8 C40 C76 116.6(7) . . ?
O28 C40 C76 117.8(7) . . ?
C36 C42 C79 124.2(7) . . ?
C36 C42 C89 118.0(7) . . ?
C89 C42 C79 117.7(7) . . ?
C55 C44 C54 122.0(7) . . ?
C57 C44 C54 120.3(7) . . ?
C57 C44 C55 117.7(7) . . ?
O1AA C48 O13 125.5(7) . . ?
O1AA C48 C35 119.7(7) . . ?
O13 C48 C35 114.7(7) . . ?
C61 C49 C81 119.2(7) . . ?
C61 C49 C83 118.3(7) . . ?
C83 C49 C81 122.5(8) . . ?
F2 C50 F12 107.1(7) . . ?
F2 C50 F16 106.5(7) . . ?
F2 C50 C79 112.4(7) . . ?
F12 C50 F16 104.9(7) . . ?
F12 C50 C79 112.0(7) . . ?
F16 C50 C79 113.3(7) . . ?
C38 C52 C78 112.4(7) . . ?
C38 C52 C80 112.3(7) . . ?
C80 C52 C78 106.0(7) . . ?
C82 C52 C38 106.3(7) . . ?
C82 C52 C78 110.7(7) . . ?
C82 C52 C80 109.3(8) . . ?
O3AA C54 C44 117.0(7) . . ?
O3AA C54 O0AA 125.3(7) . . ?
O0AA C54 C44 117.7(7) . . ?
C36 C55 C44 121.0(7) . . ?
C36 C55 H55 119.5 . . ?
C44 C55 H55 119.5 . . ?
C59 C56 C70 118.3(8) . . ?
C59 C56 C12 120.3(7) . . ?
C70 C56 C12 121.1(7) . . ?
C44 C57 H57 119.4 . . ?
C89 C57 C44 121.1(8) . . ?
C89 C57 H57 119.4 . . ?
O6 C58 O22 121.0(8) . . ?
O6 C58 C68 120.3(8) . . ?
O22 C58 C68 118.6(7) . . ?
C56 C59 H59 119.8 . . ?
C56 C59 C71 120.5(8) . . ?
C71 C59 H59 119.8 . . ?
C61 C60 H60 119.4 . . ?
C61 C60 C68 121.1(8) . . ?
C68 C60 H60 119.4 . . ?
C49 C61 H61 119.4 . . ?
C60 C61 C49 121.1(8) . . ?
C60 C61 H61 119.4 . . ?
O14 C63 O18 124.0(8) . . ?
O14 C63 C92 117.6(7) . . ?
O18 C63 C92 118.4(7) . . ?
O4 C64 C88 119.3(7) . 4_666 ?
O10 C64 O4 117.6(7) 4_566 . ?
O10 C64 C88 122.7(7) 4_566 4_666 ?
C74 C66 C79 117.2(7) . . ?
C97 C66 C74 119.3(8) . . ?
C97 C66 C79 123.5(8) . . ?
C35 C67 H67 119.8 . . ?
C35 C67 C104 120.4(8) . . ?
C104 C67 H67 119.8 . . ?
C60 C68 C58 120.8(7) . . ?
C85 C68 C58 121.4(7) . . ?
C85 C68 C60 117.8(7) . . ?
C78 C69 H69 119.4 . . ?
C78 C69 C93 121.2(8) . . ?
C93 C69 H69 119.4 . . ?
C56 C70 H70 119.1 . . ?
C100 C70 C56 121.8(8) . . ?
C100 C70 H70 119.1 . . ?
C59 C71 H71 119.1 . . ?
C59 C71 C72 121.9(8) . . ?
C72 C71 H71 119.1 . . ?
C71 C72 C81 119.5(7) . . ?
C71 C72 C100 117.1(8) . . ?
C100 C72 C81 123.2(8) . . ?
C66 C74 H74 119.9 . . ?
C66 C74 C86 120.3(8) . . ?
C86 C74 H74 119.9 . . ?
C92 C75 H75 120.0 4_466 . ?
C92 C75 C97 120.0(7) 4_466 . ?
C97 C75 H75 120.0 . . ?
C110 C76 C40 119.3(9) . . ?
C110 C76 C19 117.8(11) . . ?
C19 C76 C40 122.7(9) . . ?
C3 C76 C40 121.0(11) . . ?
C7 C76 C40 118.7(11) . . ?
C7 C76 C3 120.1(13) . . ?
C38 C77 H77 119.4 . . ?
C87 C77 C38 121.2(8) . . ?
C87 C77 H77 119.4 . . ?
C69 C78 C52 123.2(7) . . ?
C69 C78 C104 118.1(7) . . ?
C104 C78 C52 118.7(7) . . ?
C42 C79 C66 108.7(6) . . ?
C42 C79 C84 113.1(7) . . ?
C50 C79 C42 106.9(7) . . ?
C50 C79 C66 113.0(7) . . ?
C50 C79 C84 109.8(7) . . ?
C84 C79 C66 105.5(7) . . ?
F19 C80 F47 108.3(9) . . ?
F19 C80 F51 107.0(8) . . ?
F19 C80 C52 111.1(8) . . ?
F47 C80 F51 106.3(8) . . ?
F47 C80 C52 111.4(8) . . ?
F51 C80 C52 112.5(8) . . ?
C72 C81 C49 109.0(7) . . ?
C72 C81 C94 113.1(8) . . ?
C72 C81 C96 106.6(8) . . ?
C94 C81 C49 106.6(7) . . ?
C96 C81 C49 113.4(8) . . ?
C96 C81 C94 108.4(9) . . ?
F23 C82 F41 105.7(8) . . ?
F23 C82 C52 111.9(8) . . ?
F30 C82 F23 107.8(9) . . ?
F30 C82 F41 107.0(8) . . ?
F30 C82 C52 111.3(8) . . ?
F41 C82 C52 112.8(9) . . ?
C49 C83 H83 120.2 . . ?
C85 C83 C49 119.7(8) . . ?
C85 C83 H83 120.2 . . ?
F15 C84 F17 107.7(8) . . ?
F15 C84 F33 107.4(8) . . ?
F15 C84 C79 111.7(7) . . ?
F17 C84 C79 112.9(7) . . ?
F33 C84 F17 105.7(7) . . ?
F33 C84 C79 111.0(7) . . ?
C68 C85 C83 121.8(7) . . ?
C68 C85 H85 119.1 . . ?
C83 C85 H85 119.1 . . ?
C74 C86 H86 120.0 . . ?
C92 C86 C74 120.1(8) 4_466 . ?
C92 C86 H86 120.0 4_466 . ?
C77 C87 H87 120.4 . . ?
C77 C87 C98 119.3(8) . . ?
C98 C87 H87 120.4 . . ?
C13 C88 C64 118.1(10) . 4_565 ?
C13 C88 C14 124.0(12) . . ?
C14 C88 C64 117.8(9) . 4_565 ?
C4 C88 C64 124.3(11) . 4_565 ?
C4 C88 C6 118.1(14) . . ?
C6 C88 C64 117.2(10) . 4_565 ?
C42 C89 H89 119.4 . . ?
C57 C89 C42 121.2(8) . . ?
C57 C89 H89 119.4 . . ?
C113 C91 C95 117.6(11) . . ?
C113 C91 C17 116.1(12) . . ?
C17 C91 C95 124.6(11) . . ?
C2 C91 C95 120.2(13) . . ?
C9 C91 C95 118.5(14) . . ?
C9 C91 C2 121.0(16) . . ?
C75 C92 C63 121.4(7) 4_765 . ?
C86 C92 C63 119.2(8) 4_765 . ?
C86 C92 C75 119.3(7) 4_765 4_765 ?
C35 C93 C69 120.9(7) . . ?
C35 C93 H93 119.6 . . ?
C69 C93 H93 119.6 . . ?
F21 C94 C81 111.7(8) . . ?
F62 C94 F21 105.7(9) . . ?
F62 C94 C81 114.2(9) . . ?
F7 C94 F21 106.4(10) . . ?
F7 C94 F62 106.9(8) . . ?
F7 C94 C81 111.5(9) . . ?
C107 C95 C91 107.8(8) . . ?
C109 C95 C91 113.9(10) . . ?
C109 C95 C107 112.6(11) . . ?
C109 C95 C117 100.3(13) . . ?
C117 C95 C91 112.2(10) . . ?
C117 C95 C107 110.1(11) . . ?
F37 C96 F43 106.6(9) . . ?
F37 C96 F46 108.5(10) . . ?
F37 C96 C81 113.1(9) . . ?
F43 C96 C81 110.7(10) . . ?
F46 C96 F43 106.7(9) . . ?
F46 C96 C81 111.0(8) . . ?
C66 C97 C75 121.0(8) . . ?
C66 C97 H97 119.5 . . ?
C75 C97 H97 119.5 . . ?
C87 C98 C1AA 119.7(8) . . ?
C99 C98 C87 119.6(8) . . ?
C99 C98 C1AA 120.6(8) . . ?
C98 C99 H99 119.8 . . ?
C106 C99 C98 120.5(8) . . ?
C106 C99 H99 119.8 . . ?
C70 C100 C72 120.3(8) . . ?
C70 C100 H100 119.9 . . ?
C72 C100 H100 119.9 . . ?
C67 C104 C78 121.2(8) . . ?
C67 C104 H104 119.4 . . ?
C78 C104 H104 119.4 . . ?
C38 C106 H106 119.3 . . ?
C99 C106 C38 121.3(9) . . ?
C99 C106 H106 119.3 . . ?
C108 C107 C95 123.7(10) . . ?
C1 C107 C95 124.5(12) . . ?
C1 C107 C5 118.9(14) . . ?
C5 C107 C95 116.6(11) . . ?
C400 C107 C95 119.3(11) . . ?
C400 C107 C108 117.0(11) . . ?
C107 C108 H108 118.4 . . ?
C107 C108 C13 123.1(14) . . ?
C13 C108 H108 118.4 . . ?
C95 C109 F102 111.1(11) . . ?
F114 C109 C95 117.7(15) . . ?
F114 C109 F102 97.3(14) . . ?
F142 C109 C95 120.5(14) . . ?
F142 C109 F102 98.7(17) . . ?
F142 C109 F114 107.4(13) . . ?
C76 C110 H110 120.9 . . ?
C113 C110 C76 118.2(13) . . ?
C113 C110 H110 120.9 . . ?
C91 C113 C110 126.3(14) . . ?
C91 C113 H113 116.9 . . ?
C110 C113 H113 116.9 . . ?
C95 C117 F90 110.8(12) . . ?
F101 C117 F90 102.8(16) . . ?
F101 C117 C95 117.2(12) . . ?
F101 C117 F105 107.9(11) . . ?
F105 C117 F90 100.3(12) . . ?
F105 C117 C95 115.7(16) . . ?
Co3 O1 H1A 109.2 . . ?
Co3 O1 H1B 109.3 . . ?
H1A O1 H1B 109.4 . . ?
C1AA O2 Co5 146.6(6) . . ?
C0AA N28 Co5 127.3(5) . . ?
C0AA N28 N10 105.9(6) . . ?
N10 N28 Co5 126.4(5) . . ?
C54 O0AA Co2 130.4(5) . . ?
C1AA O5 Co2 118.2(5) . . ?
C8 N6 Co1 135.3(5) 1_655 . ?
C8 N6 C0AA 103.1(6) 1_655 1_655 ?
C0AA N6 Co1 121.5(5) 1_655 . ?
N6 C8 H8 124.0 1_455 . ?
N10 C8 N6 112.0(7) . 1_455 ?
N10 C8 H8 124.0 . . ?
N28 C0AA N6 112.4(6) . 1_455 ?
N28 C0AA H0AA 123.8 . . ?
N6 C0AA H0AA 123.8 1_455 . ?
N28 N10 Co2 115.3(5) . . ?
C8 N10 Co2 138.0(5) . . ?
C8 N10 N28 106.7(6) . . ?
O2 C1AA C98 119.1(8) . . ?
O2 C1AA O5 123.9(8) . . ?
O5 C1AA C98 117.0(7) . . ?
O29 C12 C56 121.3(7) . . ?
O31 C12 O29 121.0(7) . . ?
O31 C12 C56 117.4(7) . . ?
C88 C13 C108 114.8(16) . . ?
C88 C13 H13 122.6 . . ?
C108 C13 H13 122.6 . . ?
C88 C14 H14 120.3 . . ?
C400 C14 C88 119.4(14) . . ?
C400 C14 H14 120.3 . . ?
C91 C17 H17 120.3 . . ?
C19 C17 C91 119.3(15) . . ?
C19 C17 H17 120.3 . . ?
C76 C19 H19 119.7 . . ?
C17 C19 C76 120.5(15) . . ?
C17 C19 H19 119.7 . . ?
C107 C1 H1 119.0 . . ?
C107 C1 C4 122.0(19) . . ?
C4 C1 H1 119.0 . . ?
C91 C2 H2 121.1 . . ?
C7 C2 C91 118(2) . . ?
C7 C2 H2 121.1 . . ?
C76 C3 H3 120.5 . . ?
C76 C3 C9 119.0(18) . . ?
C9 C3 H3 120.5 . . ?
C88 C4 C1 122.6(19) . . ?
C88 C4 H4 118.7 . . ?
C1 C4 H4 118.7 . . ?
C107 C5 H5 121.8 . . ?
C6 C5 C107 116.3(17) . . ?
C6 C5 H5 121.8 . . ?
C107 C400 H400 119.5 . . ?
C14 C400 C107 121.1(15) . . ?
C14 C400 H400 119.5 . . ?
C88 C6 C5 121.9(18) . . ?
C88 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C76 C7 C2 119.8(19) . . ?
C76 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C91 C9 C3 122(2) . . ?
C91 C9 H9 118.9 . . ?
C3 C9 H9 118.9 . . ?
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
Co1 O13 C48 O1AA -2.1(13) 3_866 . . . ?
Co1 O13 C48 C35 -178.0(5) 3_866 . . . ?
Co1 O14 C63 O18 -25.9(13) . . . . ?
Co1 O14 C63 C92 155.7(6) . . . . ?
Co1 O22 C58 O6 -4.1(9) . . . . ?
Co1 O22 C58 C68 175.1(6) . . . . ?
Co2 N25 C26 N27 179.5(5) . . . 2_656 ?
Co2 N25 C39 N20 -179.6(5) . . . 3_766 ?
Co2 O5 C1AA C98 174.2(6) . . . . ?
Co2 O5 C1AA O2 -6.9(12) . . . . ?
Co3 O1AA C48 O13 -28.1(13) 3_866 . . . ?
Co3 O1AA C48 C35 147.7(6) 3_866 . . . ?
Co3 O18 C63 O14 10.7(14) . . . . ?
Co3 O18 C63 C92 -170.9(6) . . . . ?
Co4 O4 C64 O10 4.1(8) . . . 4_566 ?
Co4 O4 C64 C88 -169.7(6) . . . 4_666 ?
Co4 O28 C40 O8 -1.3(12) . . . . ?
Co4 O28 C40 C76 176.9(5) . . . . ?
Co4 O29 C12 O31 6.5(8) . . . . ?
Co4 O29 C12 C56 -167.7(6) . . . . ?
Co4 O31 C12 O29 -5.7(7) . . . . ?
Co4 O31 C12 C56 168.7(6) . . . . ?
Co5 O4 C64 O10 -108.6(8) . . . 4_566 ?
Co5 O4 C64 C88 77.6(9) . . . 4_666 ?
Co5 O3AA C54 C44 174.4(6) . . . . ?
Co5 O3AA C54 O0AA -5.4(14) . . . . ?
Co5 O8 C40 O28 14.8(13) . . . . ?
Co5 O8 C40 C76 -163.3(5) . . . . ?
Co5 O31 C12 O29 77.1(13) . . . . ?
Co5 O31 C12 C56 -108.5(10) . . . . ?
Co5 O2 C1AA C98 -130.9(9) . . . . ?
Co5 O2 C1AA O5 50.2(16) . . . . ?
Co5 N28 C0AA N6 -170.9(5) . . . 1_455 ?
Co5 N28 N10 Co2 -10.5(7) . . . . ?
Co5 N28 N10 C8 171.4(5) . . . . ?
F2 C50 C79 C42 -69.8(8) . . . . ?
F2 C50 C79 C66 49.7(9) . . . . ?
F2 C50 C79 C84 167.2(6) . . . . ?
O3AA C54 O0AA Co2 4.1(12) . . . . ?
O6 C58 C68 C60 -177.6(8) . . . . ?
O6 C58 C68 C85 5.3(12) . . . . ?
O8 C40 C76 C110 19.0(13) . . . . ?
O8 C40 C76 C19 -166.9(12) . . . . ?
O8 C40 C76 C3 144.4(13) . . . . ?
O8 C40 C76 C7 -31.0(15) . . . . ?
F12 C50 C79 C42 50.9(9) . . . . ?
F12 C50 C79 C66 170.4(7) . . . . ?
F12 C50 C79 C84 -72.2(8) . . . . ?
O14 C63 C92 C75 -2.5(12) . . . 4_765 ?
O14 C63 C92 C86 -179.1(8) . . . 4_765 ?
F16 C50 C79 C42 169.3(7) . . . . ?
F16 C50 C79 C66 -71.2(9) . . . . ?
F16 C50 C79 C84 46.3(9) . . . . ?
O18 C63 C92 C75 178.9(8) . . . 4_765 ?
O18 C63 C92 C86 2.4(12) . . . 4_765 ?
O22 C58 C68 C60 3.3(12) . . . . ?
O22 C58 C68 C85 -173.8(8) . . . . ?
C26 N25 C39 N20 0.2(9) . . . 3_766 ?
O28 C40 C76 C110 -159.3(11) . . . . ?
O28 C40 C76 C19 14.8(15) . . . . ?
O28 C40 C76 C3 -33.9(15) . . . . ?
O28 C40 C76 C7 150.7(13) . . . . ?
C35 C67 C104 C78 1.8(13) . . . . ?
C36 C42 C79 C50 -102.2(9) . . . . ?
C36 C42 C79 C66 135.5(8) . . . . ?
C36 C42 C79 C84 18.7(11) . . . . ?
C36 C42 C89 C57 -2.2(14) . . . . ?
C38 C52 C78 C69 -126.9(9) . . . . ?
C38 C52 C78 C104 55.5(10) . . . . ?
C38 C52 C80 F19 -46.6(10) . . . . ?
C38 C52 C80 F47 -167.4(8) . . . . ?
C38 C52 C80 F51 73.3(10) . . . . ?
C38 C52 C82 F23 -55.0(10) . . . . ?
C38 C52 C82 F30 65.7(9) . . . . ?
C38 C52 C82 F41 -174.0(7) . . . . ?
C38 C77 C87 C98 -3.7(16) . . . . ?
C39 N25 C26 N27 -0.3(9) . . . 2_656 ?
C40 C76 C110 C113 169.9(12) . . . . ?
C40 C76 C19 C17 -172.8(14) . . . . ?
C40 C76 C3 C9 -173.9(15) . . . . ?
C40 C76 C7 C2 174.9(15) . . . . ?
C42 C36 C55 C44 -1.1(13) . . . . ?
C42 C79 C84 F15 52.3(9) . . . . ?
C42 C79 C84 F17 -69.3(9) . . . . ?
C42 C79 C84 F33 172.1(7) . . . . ?
C44 C54 O0AA Co2 -175.6(5) . . . . ?
C44 C57 C89 C42 1.4(14) . . . . ?
C48 C35 C67 C104 179.2(7) . . . . ?
C48 C35 C93 C69 178.8(7) . . . . ?
C49 C81 C94 F21 -71.8(9) . . . . ?
C49 C81 C94 F62 168.3(9) . . . . ?
C49 C81 C94 F7 47.1(12) . . . . ?
C49 C81 C96 F37 -68.1(12) . . . . ?
C49 C81 C96 F43 172.3(8) . . . . ?
C49 C81 C96 F46 54.0(10) . . . . ?
C49 C83 C85 C68 -0.4(13) . . . . ?
C50 C79 C84 F15 171.5(7) . . . . ?
C50 C79 C84 F17 49.9(9) . . . . ?
C50 C79 C84 F33 -68.6(9) . . . . ?
C52 C38 C77 C87 174.7(9) . . . . ?
C52 C38 C106 C99 -170.3(10) . . . . ?
C52 C78 C104 C67 178.1(8) . . . . ?
C54 C44 C55 C36 -179.1(8) . . . . ?
C54 C44 C57 C89 179.0(8) . . . . ?
C55 C36 C42 C79 178.6(8) . . . . ?
C55 C36 C42 C89 2.1(13) . . . . ?
C55 C44 C54 O3AA -179.7(7) . . . . ?
C55 C44 C54 O0AA 0.1(12) . . . . ?
C55 C44 C57 C89 -0.3(13) . . . . ?
C56 C59 C71 C72 1.2(14) . . . . ?
C56 C70 C100 C72 2.4(16) . . . . ?
C57 C44 C54 O3AA 1.1(12) . . . . ?
C57 C44 C54 O0AA -179.2(8) . . . . ?
C57 C44 C55 C36 0.2(12) . . . . ?
C58 C68 C85 C83 173.7(8) . . . . ?
C59 C56 C70 C100 0.5(15) . . . . ?
C59 C56 C12 O29 2.4(12) . . . . ?
C59 C56 C12 O31 -172.0(8) . . . . ?
C59 C71 C72 C81 -174.1(9) . . . . ?
C59 C71 C72 C100 1.7(14) . . . . ?
C60 C68 C85 C83 -3.4(13) . . . . ?
C61 C49 C81 C72 -50.3(10) . . . . ?
C61 C49 C81 C94 72.1(10) . . . . ?
C61 C49 C81 C96 -168.8(8) . . . . ?
C61 C49 C83 C85 2.7(12) . . . . ?
C61 C60 C68 C58 -172.1(8) . . . . ?
C61 C60 C68 C85 5.1(13) . . . . ?
C64 C88 C13 C108 177.1(13) 4_565 . . . ?
C64 C88 C14 C400 -175.0(15) 4_565 . . . ?
C64 C88 C4 C1 -177.2(17) 4_565 . . . ?
C64 C88 C6 C5 174.7(17) 4_565 . . . ?
C66 C74 C86 C92 0.6(16) . . . 4_466 ?
C66 C79 C84 F15 -66.4(8) . . . . ?
C66 C79 C84 F17 171.9(7) . . . . ?
C66 C79 C84 F33 53.4(9) . . . . ?
C67 C35 C48 O1AA 17.0(11) . . . . ?
C67 C35 C48 O13 -166.8(7) . . . . ?
C67 C35 C93 C69 -0.2(12) . . . . ?
C68 C60 C61 C49 -2.8(13) . . . . ?
C69 C78 C104 C67 0.4(13) . . . . ?
C70 C56 C59 C71 -2.3(14) . . . . ?
C70 C56 C12 O29 176.8(8) . . . . ?
C70 C56 C12 O31 2.4(12) . . . . ?
C71 C72 C81 C49 -39.6(11) . . . . ?
C71 C72 C81 C94 -158.0(9) . . . . ?
C71 C72 C81 C96 83.1(10) . . . . ?
C71 C72 C100 C70 -3.5(14) . . . . ?
C72 C81 C94 F21 48.0(11) . . . . ?
C72 C81 C94 F62 -71.9(12) . . . . ?
C72 C81 C94 F7 166.8(9) . . . . ?
C72 C81 C96 F37 172.0(8) . . . . ?
C72 C81 C96 F43 52.4(11) . . . . ?
C72 C81 C96 F46 -65.9(9) . . . . ?
C74 C66 C79 C42 -42.0(11) . . . . ?
C74 C66 C79 C50 -160.5(8) . . . . ?
C74 C66 C79 C84 79.6(10) . . . . ?
C74 C66 C97 C75 2.3(15) . . . . ?
C76 C110 C113 C91 13(3) . . . . ?
C76 C3 C9 C91 -1(3) . . . . ?
C77 C38 C52 C78 24.2(12) . . . . ?
C77 C38 C52 C80 143.5(9) . . . . ?
C77 C38 C52 C82 -97.0(10) . . . . ?
C77 C38 C106 C99 1.8(15) . . . . ?
C77 C87 C98 C99 0.9(15) . . . . ?
C77 C87 C98 C1AA -175.1(9) . . . . ?
C78 C52 C80 F19 76.5(9) . . . . ?
C78 C52 C80 F47 -44.4(11) . . . . ?
C78 C52 C80 F51 -163.6(8) . . . . ?
C78 C52 C82 F23 -177.3(8) . . . . ?
C78 C52 C82 F30 -56.6(10) . . . . ?
C78 C52 C82 F41 63.7(10) . . . . ?
C78 C69 C93 C35 2.4(12) . . . . ?
C79 C42 C89 C57 -179.0(8) . . . . ?
C79 C66 C74 C86 -179.7(9) . . . . ?
C79 C66 C97 C75 179.9(8) . . . . ?
C80 C52 C78 C69 110.1(9) . . . . ?
C80 C52 C78 C104 -67.5(10) . . . . ?
C80 C52 C82 F23 66.4(10) . . . . ?
C80 C52 C82 F30 -172.9(7) . . . . ?
C80 C52 C82 F41 -52.6(10) . . . . ?
C81 C49 C61 C60 176.5(8) . . . . ?
C81 C49 C83 C85 -174.8(8) . . . . ?
C81 C72 C100 C70 172.2(9) . . . . ?
C82 C52 C78 C69 -8.3(11) . . . . ?
C82 C52 C78 C104 174.2(8) . . . . ?
C82 C52 C80 F19 -164.2(7) . . . . ?
C82 C52 C80 F47 74.9(10) . . . . ?
C82 C52 C80 F51 -44.3(10) . . . . ?
C83 C49 C61 C60 -1.1(12) . . . . ?
C83 C49 C81 C72 127.2(8) . . . . ?
C83 C49 C81 C94 -110.5(10) . . . . ?
C83 C49 C81 C96 8.7(12) . . . . ?
C87 C98 C99 C106 3.3(16) . . . . ?
C87 C98 C1AA O2 150.8(9) . . . . ?
C87 C98 C1AA O5 -30.2(13) . . . . ?
C88 C14 C400 C107 0(3) . . . . ?
C89 C42 C79 C50 74.3(9) . . . . ?
C89 C42 C79 C66 -47.9(10) . . . . ?
C89 C42 C79 C84 -164.7(8) . . . . ?
C91 C95 C107 C108 29.1(17) . . . . ?
C91 C95 C107 C1 152.5(15) . . . . ?
C91 C95 C107 C5 -31.0(16) . . . . ?
C91 C95 C107 C400 -153.0(13) . . . . ?
C91 C95 C109 F102 66.4(14) . . . . ?
C91 C95 C109 F114 -44.5(19) . . . . ?
C91 C95 C109 F142 -179.1(18) . . . . ?
C91 C95 C117 F90 -62.5(15) . . . . ?
C91 C95 C117 F101 180.0(16) . . . . ?
C91 C95 C117 F105 50.8(19) . . . . ?
C91 C17 C19 C76 -5(3) . . . . ?
C91 C2 C7 C76 -1(3) . . . . ?
C92 C75 C97 C66 -1.2(14) 4_466 . . . ?
C93 C35 C48 O1AA -162.0(7) . . . . ?
C93 C35 C48 O13 14.2(11) . . . . ?
C93 C35 C67 C104 -1.8(12) . . . . ?
C93 C69 C78 C52 180.0(7) . . . . ?
C93 C69 C78 C104 -2.5(12) . . . . ?
C94 C81 C96 F37 50.0(12) . . . . ?
C94 C81 C96 F43 -69.6(11) . . . . ?
C94 C81 C96 F46 172.1(8) . . . . ?
C95 C91 C113 C110 178.0(15) . . . . ?
C95 C91 C17 C19 176.4(14) . . . . ?
C95 C91 C2 C7 -171.9(15) . . . . ?
C95 C91 C9 C3 172.9(16) . . . . ?
C95 C107 C108 C13 -174.1(14) . . . . ?
C95 C107 C1 C4 174.1(18) . . . . ?
C95 C107 C5 C6 -177.3(16) . . . . ?
C95 C107 C400 C14 176.3(16) . . . . ?
C96 C81 C94 F21 165.9(8) . . . . ?
C96 C81 C94 F62 46.0(12) . . . . ?
C96 C81 C94 F7 -75.2(11) . . . . ?
C97 C66 C74 C86 -1.9(15) . . . . ?
C97 C66 C79 C42 140.3(9) . . . . ?
C97 C66 C79 C50 21.8(12) . . . . ?
C97 C66 C79 C84 -98.1(10) . . . . ?
C98 C99 C106 C38 -4.7(17) . . . . ?
C99 C98 C1AA O2 -25.2(13) . . . . ?
C99 C98 C1AA O5 153.8(9) . . . . ?
C100 C72 C81 C49 144.9(9) . . . . ?
C100 C72 C81 C94 26.5(13) . . . . ?
C100 C72 C81 C96 -92.4(11) . . . . ?
C106 C38 C52 C78 -163.8(8) . . . . ?
C106 C38 C52 C80 -44.5(12) . . . . ?
C106 C38 C52 C82 75.0(11) . . . . ?
C106 C38 C77 C87 2.4(15) . . . . ?
C107 C95 C109 F102 -56.6(13) . . . . ?
C107 C95 C109 F114 -167.5(13) . . . . ?
C107 C95 C109 F142 58(2) . . . . ?
C107 C95 C117 F90 57.5(13) . . . . ?
C107 C95 C117 F101 -60(2) . . . . ?
C107 C95 C117 F105 170.8(13) . . . . ?
C107 C108 C13 C88 -4(3) . . . . ?
C107 C1 C4 C88 5(4) . . . . ?
C107 C5 C6 C88 1(3) . . . . ?
C108 C107 C1 C4 -50(2) . . . . ?
C108 C107 C5 C6 69.4(19) . . . . ?
C108 C107 C400 C14 -6(3) . . . . ?
C109 C95 C107 C108 155.5(15) . . . . ?
C109 C95 C107 C1 -81.1(18) . . . . ?
C109 C95 C107 C5 95.4(16) . . . . ?
C109 C95 C107 C400 -26.6(17) . . . . ?
C109 C95 C117 F90 176.3(11) . . . . ?
C109 C95 C117 F101 59(2) . . . . ?
C109 C95 C117 F105 -70.5(16) . . . . ?
C110 C76 C19 C17 1(2) . . . . ?
C110 C76 C3 C9 -40(2) . . . . ?
C110 C76 C7 C2 72(2) . . . . ?
C113 C91 C95 C107 57.4(16) . . . . ?
C113 C91 C95 C109 -68.2(18) . . . . ?
C113 C91 C95 C117 178.7(16) . . . . ?
C113 C91 C17 C19 11(3) . . . . ?
C113 C91 C2 C7 -70(2) . . . . ?
C113 C91 C9 C3 45(2) . . . . ?
C117 C95 C107 C108 -93.5(16) . . . . ?
C117 C95 C107 C1 29.9(19) . . . . ?
C117 C95 C107 C5 -153.6(14) . . . . ?
C117 C95 C107 C400 84.3(16) . . . . ?
C117 C95 C109 F102 -173.6(11) . . . . ?
C117 C95 C109 F114 75.5(17) . . . . ?
C117 C95 C109 F142 -59(2) . . . . ?
N6 C8 N10 Co2 -176.8(6) 1_455 . . . ?
N6 C8 N10 N28 0.7(9) 1_455 . . . ?
C0AA N28 N10 Co2 176.7(5) . . . . ?
C0AA N28 N10 C8 -1.5(8) . . . . ?
N10 N28 C0AA N6 1.8(9) . . . 1_455 ?
C1AA C98 C99 C106 179.3(10) . . . . ?
C12 C56 C59 C71 172.2(8) . . . . ?
C12 C56 C70 C100 -174.0(9) . . . . ?
C13 C88 C14 C400 5(3) . . . . ?
C13 C88 C4 C1 47(3) . . . . ?
C13 C88 C6 C5 -80(2) . . . . ?
C14 C88 C13 C108 -3(2) . . . . ?
C14 C88 C4 C1 -81(3) . . . . ?
C14 C88 C6 C5 45(2) . . . . ?
C17 C91 C95 C107 -107.4(15) . . . . ?
C17 C91 C95 C109 127.0(17) . . . . ?
C17 C91 C95 C117 14(2) . . . . ?
C17 C91 C113 C110 -16(3) . . . . ?
C17 C91 C2 C7 42(2) . . . . ?
C17 C91 C9 C3 -76(2) . . . . ?
C19 C76 C110 C113 -4(2) . . . . ?
C19 C76 C3 C9 81(2) . . . . ?
C19 C76 C7 C2 -43(2) . . . . ?
C1 C107 C108 C13 49(2) . . . . ?
C1 C107 C5 C6 -1(3) . . . . ?
C1 C107 C400 C14 -73(2) . . . . ?
C2 C91 C95 C107 113.3(14) . . . . ?
C2 C91 C95 C109 -12.3(18) . . . . ?
C2 C91 C95 C117 -125.4(16) . . . . ?
C2 C91 C113 C110 71(2) . . . . ?
C2 C91 C17 C19 -39(2) . . . . ?
C2 C91 C9 C3 -1(3) . . . . ?
C3 C76 C110 C113 35.2(18) . . . . ?
C3 C76 C19 C17 -72(2) . . . . ?
C3 C76 C7 C2 -1(3) . . . . ?
C4 C88 C13 C108 -44(2) . . . . ?
C4 C88 C14 C400 73(2) . . . . ?
C4 C88 C6 C5 2(3) . . . . ?
C5 C107 C108 C13 -75(2) . . . . ?
C5 C107 C1 C4 -2(3) . . . . ?
C5 C107 C400 C14 47(2) . . . . ?
C400 C107 C108 C13 8(3) . . . . ?
C400 C107 C1 C4 75(2) . . . . ?
C400 C107 C5 C6 -46(2) . . . . ?
C6 C88 C13 C108 73.4(19) . . . . ?
C6 C88 C14 C400 -46(2) . . . . ?
C6 C88 C4 C1 -5(3) . . . . ?
C7 C76 C110 C113 -88.0(19) . . . . ?
C7 C76 C19 C17 47(2) . . . . ?
C7 C76 C3 C9 1(3) . . . . ?
C9 C91 C95 C107 -60.9(16) . . . . ?
C9 C91 C95 C109 173.4(16) . . . . ?
C9 C91 C95 C117 60.4(19) . . . . ?
C9 C91 C113 C110 -53(2) . . . . ?
C9 C91 C17 C19 82(2) . . . . ?
C9 C91 C2 C7 2(3) . . . . ?
_shelx_res_file
;
TITL CoZn in P21/n #14
REM reset to P21/n #14
CELL 1.54178 14.8692 24.8713 22.1361 90 91.6215 90
ZERR 4 0.0005 0.0008 0.0007 0 0.0023 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Co F N O
UNIT 288 152 20 96 24 69.91
SIMU 0.005 0.005 1.7 C9 C2 C7 C3
L.S. 12
PLAN 20
TEMP 23
BOND
MORE -1
BOND $H
CONF
fmap 2 53
acta
REM
REM
REM
WGHT 0.141300
FVAR 0.04360 0.40538 0.61697
CO1 3 1.521487 0.381647 0.501605 11.00000 0.02421 0.02427 =
0.01648 -0.00053 0.00110 0.00287
CO2 3 0.678267 0.472684 0.744052 11.00000 0.02759 0.01382 =
0.02224 0.00012 0.00153 -0.00223
CO3 3 1.484536 0.320651 0.353905 11.00000 0.02565 0.02177 =
0.02389 -0.00292 -0.00046 0.00144
CO4 3 0.792024 0.217053 0.750462 11.00000 0.02712 0.01539 =
0.02569 0.00234 0.00018 0.00191
CO5 3 0.688225 0.331805 0.749092 11.00000 0.02444 0.01791 =
0.02199 -0.00041 0.00137 -0.00030
F2 4 0.435488 0.334125 1.085005 11.00000 0.05426 0.03512 =
0.05095 0.00585 -0.00201 -0.00529
O1AA 6 1.415980 0.619434 0.642447 11.00000 0.03148 0.03959 =
0.03142 -0.00471 0.00157 -0.00557
O4 6 0.751020 0.271525 0.813273 11.00000 0.02900 0.03630 =
0.02477 -0.00028 -0.00586 0.00098
O3AA 6 0.613447 0.363768 0.813679 11.00000 0.03973 0.03158 =
0.02379 -0.00786 0.01083 -0.00062
O6 6 1.403840 0.352376 0.420967 11.00000 0.05015 0.05722 =
0.03480 -0.00555 0.02063 0.01518
O8 6 0.598460 0.271126 0.729532 11.00000 0.03162 0.02000 =
0.04014 0.00010 -0.00575 -0.00401
O10 6 1.384636 0.258992 0.335624 11.00000 0.04053 0.03352 =
0.02914 0.00719 -0.01484 -0.01057
F12 4 0.465959 0.418184 1.093670 11.00000 0.04990 0.03954 =
0.05002 -0.00612 -0.00974 -0.01792
O13 6 1.418378 0.572559 0.555884 11.00000 0.05028 0.04067 =
0.03123 0.00611 0.00424 -0.01478
O14 6 1.562544 0.307821 0.505373 11.00000 0.04744 0.03632 =
0.02722 -0.01011 -0.00894 0.01645
F15 4 0.238135 0.461640 0.994014 11.00000 0.04864 0.06180 =
0.06691 0.00484 -0.00017 0.01242
F16 4 0.354502 0.385311 1.139308 11.00000 0.06663 0.08295 =
0.02941 -0.00724 0.01335 -0.01924
F17 4 0.330491 0.487128 1.064313 11.00000 0.05509 0.03751 =
0.06530 -0.01861 0.01412 -0.00680
O18 6 1.553632 0.273492 0.410779 11.00000 0.04527 0.03548 =
0.03420 -0.00312 -0.00570 0.01066
F19 4 1.267553 0.416631 0.822216 11.00000 0.08141 0.08383 =
0.03963 0.00818 -0.00097 -0.01458
N20 5 1.412475 0.372526 0.295174 11.00000 0.03019 0.02461 =
0.03244 0.00197 -0.00188 -0.00410
F21 4 0.940089 0.460003 0.465464 11.00000 0.05474 0.05371 =
0.10721 0.03097 0.01551 0.01859
O22 6 1.392100 0.399282 0.504358 11.00000 0.02479 0.06455 =
0.03956 -0.00865 -0.00448 0.01006
F23 4 1.185033 0.300797 0.704609 11.00000 0.10109 0.03220 =
0.09640 0.01175 0.03383 -0.01028
N25 5 0.657897 0.551618 0.731618 11.00000 0.03330 0.01946 =
0.02317 0.00197 -0.00933 -0.00494
C26 1 0.711739 0.594296 0.743177 11.00000 0.03264 0.01344 =
0.03915 0.00114 0.00566 0.00078
AFIX 43
H26 2 0.769565 0.591512 0.760015 11.00000 -1.20000
AFIX 0
N27 5 0.826614 0.140464 0.772024 11.00000 0.02264 0.01896 =
0.02803 -0.00353 -0.00454 0.00160
O28 6 0.672266 0.193562 0.720453 11.00000 0.03667 0.02037 =
0.08612 -0.01111 -0.01944 0.00448
O29 6 0.893235 0.243643 0.696525 11.00000 0.03682 0.03570 =
0.04123 0.01322 0.01529 0.00182
F30 4 1.187201 0.352748 0.627011 11.00000 0.07201 0.04930 =
0.05333 -0.00631 0.00630 -0.02089
O31 6 0.770298 0.292083 0.685812 11.00000 0.04617 0.05375 =
0.03411 -0.00533 0.01952 0.00286
F33 4 0.220427 0.436168 1.085062 11.00000 0.05380 0.06425 =
0.06483 -0.01078 0.03349 -0.00418
C35 1 1.353577 0.531720 0.639329 11.00000 0.02155 0.04310 =
0.02103 0.00189 -0.00105 -0.00571
C36 1 0.426562 0.449911 0.953905 11.00000 0.03717 0.02803 =
0.03500 -0.00219 0.00934 -0.00519
AFIX 43
H36 2 0.403660 0.481547 0.969754 11.00000 -1.20000
AFIX 0
F37 4 0.939045 0.338111 0.339716 11.00000 0.07012 0.13824 =
0.03480 0.00177 -0.00776 -0.02480
C38 1 1.126935 0.403299 0.735103 11.00000 0.03128 0.03390 =
0.03917 0.00257 -0.00056 0.00122
C39 1 0.582229 0.575124 0.708090 11.00000 0.03909 0.01405 =
0.03409 0.00160 -0.01305 -0.00750
AFIX 43
H39 2 0.531526 0.555804 0.695513 11.00000 -1.20000
AFIX 0
C40 1 0.603121 0.222533 0.715374 11.00000 0.02821 0.02624 =
0.02201 0.01016 -0.00244 -0.00272
F41 4 1.310461 0.325397 0.668795 11.00000 0.06602 0.03921 =
0.10750 0.01310 0.02741 0.01825
C42 1 0.401868 0.401022 0.978198 11.00000 0.03566 0.03212 =
0.02962 -0.00293 0.00702 -0.00487
F43 4 0.841206 0.317174 0.404124 11.00000 0.05244 0.13607 =
0.08301 0.00238 -0.00591 -0.04876
C44 1 0.521181 0.405965 0.882531 11.00000 0.03266 0.01834 =
0.03101 -0.00146 0.00453 -0.00434
F46 4 0.969256 0.277606 0.406446 11.00000 0.07726 0.06925 =
0.06267 0.00051 -0.00473 -0.02923
F47 4 1.372290 0.382487 0.768229 11.00000 0.03074 0.11290 =
0.08587 0.04760 -0.00344 0.00219
C48 1 1.397823 0.579129 0.611198 11.00000 0.01875 0.03805 =
0.02932 -0.00362 0.00047 -0.00304
C49 1 1.070254 0.372968 0.440775 11.00000 0.03120 0.04058 =
0.01764 0.00992 0.00123 0.00502
C50 1 0.398552 0.382776 1.087117 11.00000 0.04018 0.04267 =
0.03340 -0.00173 0.00075 -0.01145
F51 4 1.268060 0.332192 0.802346 11.00000 0.05763 0.07216 =
0.07771 0.04565 -0.00098 0.01070
C52 1 1.226489 0.392487 0.721253 11.00000 0.03510 0.03568 =
0.03647 0.01100 0.00085 0.00366
C54 1 0.584673 0.407706 0.832294 11.00000 0.03082 0.03556 =
0.01758 -0.00940 0.00372 0.00233
C55 1 0.484540 0.452394 0.906615 11.00000 0.03414 0.02268 =
0.04499 0.00428 0.01025 -0.00469
AFIX 43
H55 2 0.499429 0.485661 0.890527 11.00000 -1.20000
AFIX 0
C56 1 0.883139 0.307775 0.614611 11.00000 0.03413 0.02048 =
0.04637 0.00518 0.01021 0.00171
C57 1 0.497070 0.357133 0.907678 11.00000 0.05084 0.02788 =
0.04096 -0.00348 0.01864 0.00154
AFIX 43
H57 2 0.520398 0.325440 0.892256 11.00000 -1.20000
AFIX 0
C58 1 1.356648 0.376284 0.457888 11.00000 0.04937 0.02742 =
0.02898 0.00596 0.01691 0.00626
C59 1 0.962950 0.292087 0.590607 11.00000 0.02972 0.03982 =
0.04154 0.01199 0.00291 0.00797
AFIX 43
H59 2 0.999393 0.267412 0.611242 11.00000 -1.20000
AFIX 0
C60 1 1.204431 0.406407 0.489123 11.00000 0.03605 0.04727 =
0.03566 -0.00583 0.00207 -0.00178
AFIX 43
H60 2 1.231814 0.428053 0.518549 11.00000 -1.20000
AFIX 0
C61 1 1.113732 0.403005 0.485745 11.00000 0.02843 0.04536 =
0.03093 0.00013 0.00594 0.00376
AFIX 43
H61 2 1.079836 0.421074 0.513996 11.00000 -1.20000
AFIX 0
F62 4 0.840158 0.422427 0.408944 11.00000 0.04033 0.12360 =
0.09394 0.05831 -0.00299 0.01979
C63 1 1.583952 0.273181 0.465649 11.00000 0.03486 0.04327 =
0.02801 0.00275 0.00152 -0.00049
C64 1 0.818408 0.269862 0.849899 11.00000 0.02887 0.01743 =
0.03291 0.00222 -0.00231 -0.00062
C66 1 0.270143 0.349006 1.017045 11.00000 0.03221 0.03972 =
0.03686 -0.00612 0.00728 -0.01359
C67 1 1.311456 0.535777 0.693753 11.00000 0.03026 0.03353 =
0.03180 -0.00491 -0.00051 -0.00229
AFIX 43
H67 2 1.310855 0.568527 0.714013 11.00000 -1.20000
AFIX 0
C68 1 1.257792 0.377948 0.449146 11.00000 0.02873 0.04075 =
0.02065 -0.00042 0.00236 0.00532
C69 1 1.315946 0.437345 0.637567 11.00000 0.03175 0.02320 =
0.04379 -0.00907 -0.00218 -0.00093
AFIX 43
H69 2 1.319939 0.404050 0.618709 11.00000 -1.20000
AFIX 0
C70 1 0.832022 0.346008 0.583841 11.00000 0.03071 0.04061 =
0.05696 0.01261 0.00839 0.01288
AFIX 43
H70 2 0.777974 0.357183 0.599854 11.00000 -1.20000
AFIX 0
C71 1 0.989526 0.312553 0.536262 11.00000 0.03388 0.03681 =
0.05026 0.00943 0.01848 0.00376
AFIX 43
H71 2 1.043408 0.300865 0.520442 11.00000 -1.20000
AFIX 0
C72 1 0.938146 0.350224 0.504283 11.00000 0.03089 0.03545 =
0.03424 0.00855 0.00182 -0.00600
C74 1 0.233210 0.347500 0.959313 11.00000 0.05982 0.05461 =
0.03583 0.01720 -0.01097 -0.02997
AFIX 43
H74 2 0.249925 0.373042 0.931074 11.00000 -1.20000
AFIX 0
C75 1 0.181619 0.272584 1.042875 11.00000 0.05398 0.04245 =
0.02133 0.00967 0.00092 -0.01968
AFIX 43
H75 2 0.164690 0.247411 1.071465 11.00000 -1.20000
AFIX 0
C76 1 0.520105 0.197842 0.688719 11.00000 0.03246 0.02572 =
0.03179 0.00244 -0.00425 -0.00536
C77 1 1.078473 0.441215 0.701643 11.00000 0.02873 0.05065 =
0.05573 0.02556 0.00740 0.00048
AFIX 43
H77 2 1.107787 0.461983 0.673335 11.00000 -1.20000
AFIX 0
C78 1 1.271958 0.441425 0.689947 11.00000 0.03053 0.03521 =
0.02952 0.00156 0.01026 -0.00271
C79 1 0.339115 0.394761 1.031869 11.00000 0.03644 0.03585 =
0.01957 -0.00577 0.01016 -0.01341
C80 1 1.284143 0.380975 0.779223 11.00000 0.03363 0.06406 =
0.04947 0.03011 -0.01078 0.00159
C81 1 0.966441 0.367570 0.440990 11.00000 0.03312 0.04879 =
0.04957 0.01184 0.00699 0.00350
C82 1 1.227125 0.342684 0.679934 11.00000 0.05038 0.05132 =
0.06141 0.01482 0.01606 0.00163
C83 1 1.122537 0.347078 0.398416 11.00000 0.04698 0.03914 =
0.02289 -0.00322 -0.00589 -0.00925
AFIX 43
H83 2 1.095188 0.327941 0.366823 11.00000 -1.20000
AFIX 0
C84 1 0.281621 0.445670 1.043372 11.00000 0.04578 0.05182 =
0.03772 -0.00238 0.01731 -0.00973
C85 1 1.215222 0.349958 0.403552 11.00000 0.03564 0.04604 =
0.02510 -0.00462 0.00991 0.00435
AFIX 43
H85 2 1.249600 0.332363 0.375198 11.00000 -1.20000
AFIX 0
C86 1 0.170881 0.307848 0.943040 11.00000 0.06362 0.04894 =
0.02883 0.00812 -0.02352 -0.02265
AFIX 43
H86 2 0.146527 0.306795 0.903895 11.00000 -1.20000
AFIX 0
C87 1 0.987351 0.448685 0.709628 11.00000 0.03792 0.04408 =
0.06246 0.03065 0.00791 0.00352
AFIX 43
H87 2 0.956382 0.475617 0.688618 11.00000 -1.20000
AFIX 0
C88 1 0.312917 0.203445 0.409133 11.00000 0.04488 0.03184 =
0.02203 0.00920 -0.00952 -0.01266
C89 1 0.439547 0.354797 0.954789 11.00000 0.05703 0.01755 =
0.04582 0.00513 0.02030 -0.00715
AFIX 43
H89 2 0.425493 0.321597 0.971391 11.00000 -1.20000
AFIX 0
F90 4 0.346044 0.056501 0.564217 11.00000 0.23908 0.04317 =
0.13495 -0.01134 -0.13375 -0.00929
C91 1 0.366892 0.157550 0.629937 11.00000 0.06448 0.04623 =
0.04291 0.02101 -0.01786 -0.01859
C92 1 1.645365 0.229686 0.484743 11.00000 0.04213 0.02234 =
0.03460 -0.00173 0.00462 0.00983
C93 1 1.355345 0.481986 0.611338 11.00000 0.03265 0.03829 =
0.02858 -0.00473 0.00878 0.00381
AFIX 43
H93 2 1.383265 0.478385 0.574489 11.00000 -1.20000
AFIX 0
C94 1 0.927760 0.422775 0.421717 11.00000 0.03256 0.08108 =
0.05977 0.03044 -0.00268 0.00996
C95 1 0.282358 0.139808 0.591191 11.00000 0.06034 0.06358 =
0.05095 0.01068 -0.01423 -0.03048
C96 1 0.929474 0.324844 0.396723 11.00000 0.03741 0.10287 =
0.04986 0.01587 0.00001 -0.02764
C97 1 0.243092 0.312309 1.058521 11.00000 0.04549 0.05069 =
0.01936 0.00780 -0.00536 -0.02708
AFIX 43
H97 2 0.266316 0.314009 1.097927 11.00000 -1.20000
AFIX 0
C98 1 0.942506 0.415401 0.749502 11.00000 0.02756 0.03715 =
0.04971 -0.00272 0.00688 -0.00322
C99 1 0.989941 0.375978 0.781056 11.00000 0.03696 0.05462 =
0.07099 0.03294 0.01636 -0.00504
AFIX 43
H99 2 0.959660 0.352534 0.806129 11.00000 -1.20000
AFIX 0
C100 1 0.858778 0.367790 0.530578 11.00000 0.03831 0.04867 =
0.05612 0.02256 0.01054 0.01530
AFIX 43
H100 2 0.824133 0.394385 0.511724 11.00000 -1.20000
AFIX 0
F101 4 0.201711 0.063858 0.560203 11.00000 0.19322 0.07976 =
0.26875 0.04050 -0.17082 -0.08286
F102 4 0.191147 0.214052 0.613516 11.00000 0.06154 0.24386 =
0.08259 -0.03750 -0.01081 0.04967
C104 1 1.270121 0.491539 0.718423 11.00000 0.04205 0.04281 =
0.03229 -0.00661 0.01186 -0.00315
AFIX 43
H104 2 1.240517 0.495154 0.754650 11.00000 -1.20000
AFIX 0
F105 4 0.272099 0.059731 0.645402 11.00000 0.13884 0.18372 =
0.16501 0.14307 -0.04318 -0.08085
C106 1 1.080117 0.371337 0.775649 11.00000 0.03836 0.06267 =
0.04815 0.02840 0.00538 -0.00192
AFIX 43
H106 2 1.111548 0.346400 0.799369 11.00000 -1.20000
AFIX 0
C107 1 0.294793 0.160421 0.525164 11.00000 0.05504 0.03637 =
0.03944 0.01155 -0.01143 -0.01361
PART 1
C108 1 0.380230 0.167674 0.498815 -21.00000 0.06379 0.07926 =
0.03791 0.02252 -0.03933 -0.00307
AFIX 43
H108 2 0.431371 0.156652 0.520586 -21.00000 -1.20000
AFIX 0
PART 0
C109 1 0.199999 0.156264 0.615166 11.00000 0.04297 0.19722 =
0.06772 -0.00965 -0.00571 -0.06229
PART 1
C110 1 0.453966 0.230406 0.664804 31.00000 0.03938 0.03647 =
0.04283 0.00509 -0.01494 -0.00725
AFIX 43
H110 2 0.455943 0.267431 0.670563 31.00000 -1.20000
AFIX 0
C113 1 0.384918 0.207053 0.632226 31.00000 0.05848 0.03828 =
0.05318 0.01153 -0.03077 -0.00713
AFIX 43
H113 2 0.347666 0.229883 0.609576 31.00000 -1.20000
AFIX 0
PART 0
F114 4 0.189169 0.149909 0.675218 11.00000 0.24178 0.27137 =
0.09484 -0.02752 0.08484 -0.15620
C117 1 0.270494 0.083058 0.591228 11.00000 0.10473 0.06565 =
0.14124 0.05668 -0.07379 -0.05422
F142 4 0.124914 0.143799 0.588364 11.00000 0.05094 0.44450 =
0.30774 -0.23956 0.00853 -0.07145
O1 6 1.546673 0.284100 0.279829 11.00000 0.04177 0.04573 =
0.03371 -0.01104 -0.00454 0.01280
AFIX 7
H1A 2 1.506463 0.270525 0.256392 11.00000 -1.50000
H1B 2 1.581909 0.259423 0.292639 11.00000 -1.50000
AFIX 0
O2 6 0.798866 0.379949 0.768832 11.00000 0.03702 0.04577 =
0.05560 0.00224 -0.00229 -0.01542
N28 5 0.628083 0.377357 0.677254 11.00000 0.03940 0.01469 =
0.02551 0.00232 0.00108 0.00066
O0AA 6 0.605282 0.453597 0.811422 11.00000 0.05155 0.02465 =
0.03334 0.00316 0.01473 -0.00934
O5 6 0.808408 0.466335 0.745281 11.00000 0.02632 0.04628 =
0.06885 0.00931 0.00384 -0.00120
N6 5 1.570778 0.398379 0.587005 11.00000 0.03634 0.01785 =
0.02504 -0.00146 0.00955 0.00560
F7 4 0.967457 0.441554 0.373669 11.00000 0.06089 0.11169 =
0.09364 0.07463 0.02607 0.02264
C8 1 0.596354 0.442905 0.616777 11.00000 0.04616 0.02744 =
0.01898 -0.00755 -0.00978 -0.00348
AFIX 43
H8 2 0.590801 0.477458 0.601051 11.00000 -1.20000
AFIX 0
C0AA 1 0.590788 0.358872 0.626855 11.00000 0.03590 0.01934 =
0.01736 0.00109 -0.00871 -0.00646
AFIX 43
H0AA 2 0.579492 0.322644 0.619526 11.00000 -1.20000
AFIX 0
N10 5 0.630373 0.431964 0.671067 11.00000 0.04084 0.01376 =
0.03017 0.00289 0.00037 0.00130
C1AA 1 0.842799 0.420190 0.754814 11.00000 0.03318 0.02842 =
0.04349 -0.00666 -0.00066 -0.01292
C12 1 0.848580 0.280284 0.669910 11.00000 0.03882 0.03268 =
0.01696 -0.01287 -0.00538 0.00053
PART 1
C13 1 0.391274 0.191421 0.439673 -21.00000 0.06815 0.03966 =
0.04082 0.01671 -0.03701 -0.00935
AFIX 43
H13 2 0.447472 0.197950 0.423787 -21.00000 -1.20000
AFIX 0
C14 1 0.226378 0.192117 0.430908 -21.00000 0.03568 0.08415 =
0.02071 0.01054 -0.00185 -0.00544
AFIX 43
H14 2 0.175323 0.198838 0.406853 -21.00000 -1.20000
AFIX 0
C17 1 0.436051 0.122097 0.651147 31.00000 0.10456 0.04828 =
0.06776 -0.00195 -0.00619 -0.05302
AFIX 43
H17 2 0.431419 0.085315 0.644170 31.00000 -1.20000
AFIX 0
C19 1 0.509732 0.142782 0.682039 31.00000 0.05829 0.03090 =
0.05920 -0.00363 -0.02051 -0.00877
AFIX 43
H19 2 0.552943 0.119638 0.698580 31.00000 -1.20000
AFIX 0
PART 0
PART 2
C1 1 0.258784 0.137265 0.476121 21.00000 0.02438 0.03820 =
0.02123 -0.00818 -0.01525 -0.00103
AFIX 43
H1 2 0.228310 0.104858 0.480083 21.00000 -1.20000
AFIX 0
C2 1 0.358008 0.197420 0.678683 -31.00000 0.05342 0.02174 =
0.02318 0.00112 -0.00838 -0.00749
AFIX 43
H2 2 0.301781 0.209170 0.690477 -31.00000 -1.20000
AFIX 0
C3 1 0.524730 0.158712 0.643185 -31.00000 0.03495 0.02182 =
0.03357 0.01109 0.01469 -0.00396
AFIX 43
H3 2 0.580028 0.145202 0.631745 -31.00000 -1.20000
AFIX 0
C4 1 0.265271 0.160000 0.419070 21.00000 0.03185 0.06619 =
0.01760 0.00408 -0.00984 -0.00004
AFIX 43
H4 2 0.234693 0.143835 0.386650 21.00000 -1.20000
AFIX 0
C5 1 0.345255 0.209905 0.518547 21.00000 0.04374 0.03121 =
0.02393 -0.00268 -0.00859 -0.02051
AFIX 43
H5 2 0.371165 0.227680 0.551652 21.00000 -1.20000
AFIX 0
PART 0
PART 1
C400 1 0.218427 0.170970 0.488259 -21.00000 0.04501 0.07276 =
0.03075 0.00201 -0.02005 -0.01619
AFIX 43
H400 2 0.161573 0.163605 0.502648 -21.00000 -1.20000
AFIX 0
PART 0
PART 2
C6 1 0.352886 0.229657 0.458856 21.00000 0.05730 0.02642 =
0.02980 0.01708 -0.00478 0.00664
AFIX 43
H6 2 0.385457 0.260991 0.452594 21.00000 -1.20000
AFIX 0
C7 1 0.436882 0.216959 0.706566 -31.00000 0.05414 0.01892 =
0.02256 -0.00051 -0.00826 -0.00973
AFIX 43
H7 2 0.433845 0.242658 0.736958 -31.00000 -1.20000
AFIX 0
C9 1 0.444288 0.140213 0.615074 -31.00000 0.03440 0.02167 =
0.03054 0.01142 0.01545 -0.00453
AFIX 43
H9 2 0.447541 0.114528 0.584681 -31.00000 -1.20000
AFIX 0
PART 0
O11 6 1.711896 0.307381 0.292454 0.47741 0.12781 0.14280 =
0.18931 -0.04901 0.02032 0.01221
HKLF 4
REM CoZn in P21/n #14
REM R1 = 0.0776 for 8518 Fo > 4sig(Fo) and 0.1298 for all 13811 data
REM 1202 parameters refined using 12 restraints
END
WGHT 0.1412 0.0000
REM Highest difference peak 0.867, deepest hole -0.730, 1-sigma level 0.132
Q1 1 1.6047 0.3175 0.2416 11.00000 0.05 0.87
Q2 1 0.3902 0.0190 0.5909 11.00000 0.05 0.70
Q3 1 0.4574 0.0569 0.5426 11.00000 0.05 0.69
Q4 1 0.3513 0.0328 0.4969 11.00000 0.05 0.68
Q5 1 0.0989 0.3391 0.9368 11.00000 0.05 0.55
Q6 1 0.7831 0.1996 0.8073 11.00000 0.05 0.55
Q7 1 1.3791 0.3947 0.3824 11.00000 0.05 0.52
Q8 1 1.4173 0.3433 0.4992 11.00000 0.05 0.50
Q9 1 0.1299 0.1226 0.6004 11.00000 0.05 0.49
Q10 1 0.8225 0.4801 0.6375 11.00000 0.05 0.49
Q11 1 0.7786 0.2386 0.8183 11.00000 0.05 0.46
Q12 1 1.5005 0.2997 0.3077 11.00000 0.05 0.45
Q13 1 1.5247 0.4021 0.4596 11.00000 0.05 0.45
Q14 1 0.5037 0.3772 1.1103 11.00000 0.05 0.45
Q15 1 1.5025 0.3015 0.1767 11.00000 0.05 0.44
Q16 1 0.2376 0.3019 0.8991 11.00000 0.05 0.44
Q17 1 1.4639 0.3450 0.4023 11.00000 0.05 0.44
Q18 1 0.9032 0.4394 0.6017 11.00000 0.05 0.43
Q19 1 0.3248 0.0204 0.5999 11.00000 0.05 0.43
Q20 1 0.9033 0.3001 0.8601 11.00000 0.05 0.43
;
_shelx_res_checksum 28824
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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# Audit and citation data items may have been added by the CCDC.
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data_JG41_0m
_database_code_depnum_ccdc_archive 'CCDC 1429141'
_audit_update_record
;
2015-10-01 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_audit_creation_date 2015-08-20
_audit_creation_method 'Materials Studio'
_symmetry_space_group_name_H-M PNMA
_symmetry_Int_Tables_number 62
_symmetry_cell_setting orthorhombic
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,-y,z+1/2
-x,y+1/2,-z
x+1/2,-y+1/2,-z+1/2
-x,-y,-z
x+1/2,y,-z+1/2
x,-y+1/2,z
-x+1/2,y+1/2,z+1/2
_cell_length_a 7.5987
_cell_length_b 10.0166
_cell_length_c 17.4578
_cell_angle_alpha 90.0000
_cell_angle_beta 90.0000
_cell_angle_gamma 90.0000
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
N1 N 0.20604 0.41247 0.63896 0.05000 Uiso 1.00
N2 N 0.32756 0.59813 0.69395 0.05000 Uiso 1.00
C3 C 0.08357 0.48079 0.67616 0.05000 Uiso 1.00
C4 C 0.36604 0.48374 0.64825 0.05000 Uiso 1.00
N5 N 0.15143 0.59496 0.70966 0.05000 Uiso 1.00
H6 H -0.05647 0.44241 0.67723 0.05000 Uiso 1.00
H7 H 0.49075 0.44421 0.62085 0.05000 Uiso 1.00
Co8 Co 0.15613 0.25000 0.58217 0.05000 Uiso 1.00
N9 N 0.21997 0.25000 0.47267 0.05000 Uiso 1.00
O10 O -0.13543 0.25000 0.58632 0.05000 Uiso 1.00
C11 C -0.27637 0.25000 0.61591 0.05000 Uiso 1.00
C12 C 0.38573 0.25000 0.43735 0.05000 Uiso 1.00
H13 H 0.50631 0.25000 0.47225 0.05000 Uiso 1.00
H14 H -0.06457 0.25000 0.43976 0.05000 Uiso 1.00
C15 C 0.59742 0.25000 0.57129 0.05000 Uiso 1.00
Co16 Co 0.51066 0.75000 0.74155 0.05000 Uiso 1.00
N17 N 0.83176 0.75000 0.65007 0.05000 Uiso 1.00
N18 N 0.65762 0.75000 0.64126 0.05000 Uiso 1.00
C19 C 0.92724 0.75000 0.58268 0.05000 Uiso 1.00
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_ccdc_geom_bond_type
N1 C3 1.325 . A
N1 C4 1.419 . A
N1 Co8 1.943 . S
N2 C4 1.426 . A
N2 N5 1.367 . A
C3 N5 1.384 . A
C3 H6 1.132 . S
C4 H7 1.133 . S
Co8 N1 1.943 7 S
Co8 N9 1.972 . S
Co8 O10 2.217 . S
N9 C12 1.402 . A
N9 C19 1.478 3_646 A
O10 C11 1.189 . S
C11 C15 1.236 1_455 S
C12 N18 1.411 3_646 A
C12 H13 1.100 . S
H14 C19 1.115 3_646 S
C15 C11 1.236 1_655 S
N17 N18 1.332 . A
N17 C19 1.382 . A
N18 C12 1.411 3_656 A
C19 N9 1.478 3_656 A
C19 H14 1.115 3_656 S
_refine_special_details 'Rietlveld refinement-PXRD data'