# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1885053'
loop_
_audit_author_name
_audit_author_address
'Fengcai Li'
;Zhengzhou University of Light Industry
China
;
_audit_update_record
;
2018-12-14 deposited with the CCDC. 2019-04-01 downloaded from the CCDC.
;
_audit_creation_date 2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H26 Co2 Cu2 Mo10 N4 O45, C16 H22 Cu N4 O5'
_chemical_formula_sum 'C32 H48 Co2 Cu3 Mo10 N8 O50'
_chemical_formula_weight 2612.66
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.1598(5)
_cell_length_b 14.1021(6)
_cell_length_c 23.8608(12)
_cell_angle_alpha 78.079(4)
_cell_angle_beta 82.282(4)
_cell_angle_gamma 83.825(3)
_cell_volume 3953.6(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9029
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.3700
_cell_measurement_theta_min 3.3380
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.820
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.70871
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear dark green'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 2.195
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2514
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.23
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0604
_diffrn_reflns_av_unetI/netI 0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 37927
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.500
_diffrn_reflns_theta_min 3.008
_diffrn_ambient_temperature 298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'multiwire proportional'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 11050
_reflns_number_total 16348
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.606
_refine_diff_density_min -2.842
_refine_diff_density_rms 0.275
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 954
_refine_ls_number_reflns 16348
_refine_ls_number_restraints 1020
_refine_ls_R_factor_all 0.1279
_refine_ls_R_factor_gt 0.0923
_refine_ls_restrained_S_all 1.036
_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^)+(0.0871P)^2^+116.2981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2229
_refine_ls_wR_factor_ref 0.2481
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim O50 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16
\\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24
\\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32
\\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40
\\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O41 \\sim O42 \\sim O47 \\sim O48
\\sim O49: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
O50(H50a,H50b), O43(H43a,H43b), O44(H44a,H44b), O45(H45a,H45b), O46(H46a,
H46b), O47(Hp,Hq), O48(Hr,Hs), O49(Ht,Hu)
3.b Secondary CH2 refined with riding coordinates:
C7(H7a,H7b), C8(H8a,H8b), C15(H15a,H15b), C16(H16a,H16b), C23(Hd,He), C24(Hf,
Hg), C25(Hh,Hi), C26(Hj,Hk)
3.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C17(H),
C18(Ha), C19(Hb), C20(Hc), C29(Hl), C30(Hm), C31(Hn), C32(Ho)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3777(11) 0.4434(10) 0.9110(6) 0.031(3) Uani 1 1 d . . . . .
H1 H 0.3868 0.5075 0.8928 0.037 Uiso 1 1 calc R . . . .
C2 C 0.4529(13) 0.2837(12) 0.9429(6) 0.038(4) Uani 1 1 d . . . . .
H2 H 0.5141 0.2380 0.9454 0.045 Uiso 1 1 calc R . . . .
C3 C 0.3521(11) 0.2559(10) 0.9661(6) 0.030(3) Uani 1 1 d . . . . .
H3 H 0.3448 0.1924 0.9859 0.035 Uiso 1 1 calc R . . . .
C4 C 0.2595(13) 0.3205(11) 0.9611(7) 0.038(4) Uani 1 1 d . . . . .
H4 H 0.1890 0.3011 0.9759 0.046 Uiso 1 1 calc R . . . .
C5 C 0.2739(11) 0.4160(11) 0.9331(6) 0.031(3) Uani 1 1 d . . . . .
C6 C 0.1755(13) 0.4924(12) 0.9207(7) 0.040(4) Uani 1 1 d . . . . .
C7 C -0.0022(12) 0.5733(13) 0.9477(7) 0.042(4) Uani 1 1 d . . . . .
H7A H -0.0037 0.5897 0.9062 0.051 Uiso 1 1 calc R . . . .
H7B H -0.0011 0.6331 0.9616 0.051 Uiso 1 1 calc R . . . .
C8 C 0.1036(11) 0.4766(11) 1.0245(6) 0.031(3) Uani 1 1 d . . . . .
H8A H 0.1085 0.5327 1.0414 0.037 Uiso 1 1 calc R . . . .
H8B H 0.1695 0.4326 1.0314 0.037 Uiso 1 1 calc R . . . .
C9 C 0.6587(12) 0.3622(10) 0.9997(6) 0.031(3) Uani 1 1 d . . . . .
H9 H 0.5949 0.4036 1.0051 0.038 Uiso 1 1 calc R . . . .
C10 C 0.7926(11) 0.2919(11) 0.9379(6) 0.031(3) Uani 1 1 d . . . . .
H10 H 0.8212 0.2842 0.9008 0.038 Uiso 1 1 calc R . . . .
C11 C 0.7136(12) 0.3186(11) 1.0473(7) 0.035(3) Uani 1 1 d . . . . .
H11 H 0.6844 0.3279 1.0840 0.042 Uiso 1 1 calc R . . . .
C12 C 0.8121(14) 0.2614(11) 1.0394(7) 0.042(4) Uani 1 1 d . . . . .
H12 H 0.8511 0.2332 1.0705 0.051 Uiso 1 1 calc R . . . .
C13 C 0.8512(12) 0.2471(10) 0.9846(6) 0.033(3) Uani 1 1 d . . . . .
C14 C 0.9646(13) 0.1946(12) 0.9685(7) 0.041(4) Uani 1 1 d . . . . .
C15 C 1.0952(14) 0.0528(12) 0.9837(9) 0.051(4) Uani 1 1 d . . . . .
H15A H 1.1288 0.0437 1.0193 0.061 Uiso 1 1 calc R . . . .
H15B H 1.1406 0.0941 0.9540 0.061 Uiso 1 1 calc R . . . .
C16 C 1.0947(16) -0.0410(12) 0.9676(9) 0.054(5) Uani 1 1 d . . . . .
H16A H 1.1687 -0.0744 0.9679 0.065 Uiso 1 1 calc R . . . .
H16B H 1.0738 -0.0316 0.9288 0.065 Uiso 1 1 calc R . . . .
Co1 Co 0.76810(14) 0.65662(12) 0.67021(8) 0.0226(4) Uani 1 1 d . . . . .
Co2 Co 0.78880(15) 0.73535(13) 0.76602(8) 0.0236(4) Uani 1 1 d . . . . .
Cu1 Cu 0.62048(14) 0.41178(13) 0.87662(7) 0.0297(4) Uani 1 1 d . . . . .
Cu2 Cu 0.1685(3) 0.4806(3) 0.79579(14) 0.0862(9) Uani 1 1 d . . . . .
Mo1 Mo 0.58366(9) 0.61179(8) 0.76505(5) 0.0235(3) Uani 1 1 d . . . . .
Mo2 Mo 0.61599(10) 0.68637(9) 0.88226(5) 0.0282(3) Uani 1 1 d . . . . .
Mo3 Mo 0.81639(11) 0.82785(9) 0.88003(6) 0.0328(3) Uani 1 1 d . . . . .
Mo4 Mo 0.99548(11) 0.86921(10) 0.76378(6) 0.0352(3) Uani 1 1 d . . . . .
Mo5 Mo 0.97345(10) 0.77080(10) 0.65265(5) 0.0316(3) Uani 1 1 d . . . . .
Mo6 Mo 0.72392(10) 0.89206(9) 0.66526(5) 0.0290(3) Uani 1 1 d . . . . .
Mo7 Mo 0.71955(10) 0.80435(9) 0.54889(5) 0.0287(3) Uani 1 1 d . . . . .
Mo8 Mo 0.75096(11) 0.56528(9) 0.55469(5) 0.0305(3) Uani 1 1 d . . . . .
Mo9 Mo 0.80064(10) 0.42356(9) 0.67764(5) 0.0278(3) Uani 1 1 d . . . . .
Mo10 Mo 0.84436(9) 0.52134(8) 0.78583(5) 0.0238(3) Uani 1 1 d . . . . .
N1 N 0.4681(9) 0.3776(9) 0.9155(5) 0.033(3) Uani 1 1 d . . . . .
N2 N 0.0993(10) 0.5082(10) 0.9615(5) 0.036(3) Uani 1 1 d . . . . .
N3 N 0.6945(9) 0.3465(9) 0.9461(5) 0.029(3) Uani 1 1 d . . . . .
N4 N 0.9855(10) 0.1006(10) 0.9915(6) 0.042(3) Uani 1 1 d . . . . .
O1 O 0.4906(8) 0.6309(7) 0.7163(4) 0.036(2) Uani 1 1 d . U . . .
O50 O 0.6301(11) 0.2733(10) 0.8370(5) 0.058(3) Uani 1 1 d . U . . .
H50A H 0.6128 0.2231 0.8638 0.088 Uiso 1 1 d GR . . . .
H50B H 0.6988 0.2570 0.8239 0.088 Uiso 1 1 d GR . . . .
O2 O 0.5552(8) 0.4992(7) 0.8106(4) 0.0314(17) Uani 1 1 d . U . . .
O3 O 0.5306(8) 0.6930(7) 0.8166(4) 0.0294(16) Uani 1 1 d . U . . .
O4 O 0.7316(8) 0.6226(7) 0.8123(4) 0.0286(14) Uani 1 1 d . U . . .
O5 O 0.5924(9) 0.5701(7) 0.9178(4) 0.037(2) Uani 1 1 d . U . . .
O6 O 0.5244(9) 0.7594(8) 0.9159(5) 0.042(2) Uani 1 1 d . U . . .
O7 O 0.7502(8) 0.7055(7) 0.9094(4) 0.0325(17) Uani 1 1 d . U . . .
O8 O 0.6943(8) 0.8084(7) 0.8173(4) 0.0281(15) Uani 1 1 d . U . . .
O9 O 0.7232(9) 0.9072(8) 0.9117(5) 0.041(2) Uani 1 1 d . U . . .
O10 O 0.9239(9) 0.8027(8) 0.9213(5) 0.044(2) Uani 1 1 d . U . . .
O11 O 0.8765(8) 0.9200(7) 0.8140(5) 0.0370(18) Uani 1 1 d . U . . .
O12 O 0.9049(8) 0.7405(7) 0.8133(4) 0.0316(16) Uani 1 1 d . U . . .
O13 O 1.0988(9) 0.8490(9) 0.8062(5) 0.048(3) Uani 1 1 d . U . . .
O14 O 1.0182(10) 0.9769(9) 0.7160(5) 0.051(3) Uani 1 1 d . U . . .
O15 O 0.8472(8) 0.8444(7) 0.7136(4) 0.0303(15) Uani 1 1 d . U . . .
O16 O 1.0509(8) 0.7728(7) 0.7163(4) 0.0353(18) Uani 1 1 d . U . . .
O17 O 1.0144(9) 0.8720(8) 0.6066(5) 0.043(2) Uani 1 1 d . U . . .
O18 O 1.0445(8) 0.6741(8) 0.6249(5) 0.042(2) Uani 1 1 d . U . . .
O19 O 0.8742(8) 0.6505(7) 0.7217(4) 0.0286(15) Uani 1 1 d . U . . .
O20 O 0.6792(7) 0.7327(7) 0.7174(4) 0.0269(14) Uani 1 1 d . U . . .
O21 O 0.6261(9) 0.9360(7) 0.7146(5) 0.040(2) Uani 1 1 d . U . . .
O22 O 0.7877(9) 0.9914(7) 0.6270(5) 0.040(2) Uani 1 1 d . U . . .
O23 O 0.8267(8) 0.7737(7) 0.6251(4) 0.0292(15) Uani 1 1 d . U . . .
O24 O 0.6412(8) 0.8677(7) 0.6100(4) 0.0328(17) Uani 1 1 d . U . . .
O25 O 0.8047(9) 0.8914(8) 0.5127(5) 0.042(2) Uani 1 1 d . U . . .
O26 O 0.6107(8) 0.8143(8) 0.5088(4) 0.038(2) Uani 1 1 d . U . . .
O27 O 0.8071(8) 0.6916(7) 0.5258(4) 0.0338(17) Uani 1 1 d . U . . .
O28 O 0.8550(8) 0.5664(7) 0.6276(4) 0.0280(15) Uani 1 1 d . U . . .
O29 O 0.6664(7) 0.6679(7) 0.6126(4) 0.0270(15) Uani 1 1 d . U . . .
O30 O 0.8560(9) 0.4983(8) 0.5213(5) 0.043(2) Uani 1 1 d . U . . .
O31 O 0.6411(9) 0.5708(8) 0.5158(4) 0.041(2) Uani 1 1 d . U . . .
O32 O 0.6998(8) 0.4702(7) 0.6220(4) 0.0322(17) Uani 1 1 d . U . . .
O33 O 0.8977(9) 0.3543(7) 0.6420(4) 0.038(2) Uani 1 1 d . U . . .
O34 O 0.7241(9) 0.3407(7) 0.7247(4) 0.036(2) Uani 1 1 d . U . . .
O35 O 0.9035(8) 0.4505(7) 0.7301(4) 0.0293(16) Uani 1 1 d . U . . .
O36 O 0.7160(7) 0.5460(6) 0.7219(4) 0.0258(14) Uani 1 1 d . U . . .
O37 O 0.9604(8) 0.5336(8) 0.8183(4) 0.035(2) Uani 1 1 d . U . . .
O38 O 0.7705(8) 0.4349(7) 0.8346(4) 0.0288(17) Uani 1 1 d . U . . .
O39 O 1.0340(9) 0.2428(9) 0.9356(5) 0.054(3) Uani 1 1 d . U . . .
O40 O 0.1695(10) 0.5303(11) 0.8696(5) 0.063(3) Uani 1 1 d . U . . .
O43 O 0.1971(13) 0.6123(11) 0.7554(6) 0.077(4) Uani 1 1 d . U . . .
H43A H 0.2702 0.6250 0.7517 0.115 Uiso 1 1 d GR . . . .
H43B H 0.1647 0.6587 0.7754 0.115 Uiso 1 1 d GR . . . .
O44 O 0.3471(15) 0.4298(13) 0.7780(8) 0.093(4) Uani 1 1 d . U . . .
H44A H 0.3732 0.4238 0.7379 0.139 Uiso 1 1 d GR . . . .
H44B H 0.3675 0.3625 0.7967 0.139 Uiso 1 1 d GR . . . .
O45 O 0.1335(14) 0.4449(14) 0.7249(7) 0.090(4) Uani 1 1 d . U . . .
H45A H 0.1610 0.3797 0.7189 0.135 Uiso 1 1 d GR . . . .
H45B H 0.1677 0.4812 0.6882 0.135 Uiso 1 1 d GR . . . .
O46 O 0.1265(17) 0.3507(14) 0.8348(8) 0.103(5) Uani 1 1 d . U . . .
H46A H 0.1501 0.3042 0.8137 0.154 Uiso 1 1 d GR . . . .
H46B H 0.0515 0.3454 0.8400 0.154 Uiso 1 1 d GR . . . .
C17 C 0.7004(14) 0.2421(14) 0.6088(8) 0.050(4) Uani 1 1 d . . . . .
H H 0.7137 0.2346 0.6470 0.060 Uiso 1 1 calc R . . . .
C18 C 0.7630(15) 0.2358(13) 0.5152(7) 0.044(4) Uani 1 1 d . . . . .
HA H 0.8212 0.2274 0.4867 0.053 Uiso 1 1 calc R . . . .
C19 C 0.5936(16) 0.2634(15) 0.5957(9) 0.060(5) Uani 1 1 d . . . . .
HB H 0.5358 0.2738 0.6241 0.072 Uiso 1 1 calc R . . . .
C20 C 0.5735(16) 0.2689(17) 0.5407(10) 0.069(6) Uani 1 1 d . . . . .
HC H 0.5016 0.2846 0.5304 0.083 Uiso 1 1 calc R . . . .
C21 C 0.6576(13) 0.2517(12) 0.5015(8) 0.045(4) Uani 1 1 d . . . . .
C22 C 0.6409(16) 0.2629(15) 0.4382(9) 0.058(5) Uani 1 1 d . . . . .
C23 C 0.6822(12) 0.2082(11) 0.3462(7) 0.041(4) Uani 1 1 d . . . . .
HD H 0.6551 0.2749 0.3318 0.050 Uiso 1 1 calc R . . . .
HE H 0.7584 0.1986 0.3288 0.050 Uiso 1 1 calc R . . . .
C24 C 0.6161(15) 0.1446(13) 0.3289(7) 0.050(4) Uani 1 1 d . . . . .
HF H 0.6257 0.1526 0.2872 0.061 Uiso 1 1 calc R . . . .
HG H 0.5380 0.1596 0.3413 0.061 Uiso 1 1 calc R . . . .
C25 C 0.7161(15) 0.0913(12) 0.4357(8) 0.047(4) Uani 1 1 d . . . . .
HH H 0.7062 0.0835 0.4774 0.057 Uiso 1 1 calc R . . . .
HI H 0.7941 0.0759 0.4234 0.057 Uiso 1 1 calc R . . . .
C26 C 0.6454(13) 0.0241(12) 0.4172(7) 0.043(4) Uani 1 1 d . . . . .
HJ H 0.6718 -0.0430 0.4310 0.052 Uiso 1 1 calc R . . . .
HK H 0.5687 0.0341 0.4337 0.052 Uiso 1 1 calc R . . . .
C27 C 0.6918(16) -0.0201(13) 0.3230(8) 0.051(4) Uani 1 1 d . . . . .
C28 C 0.7411(15) -0.1172(14) 0.3495(7) 0.047(4) Uani 1 1 d . . . . .
C29 C 0.8449(13) -0.1254(12) 0.3711(7) 0.041(4) Uani 1 1 d . . . . .
HL H 0.8769 -0.0689 0.3723 0.050 Uiso 1 1 calc R . . . .
C30 C 0.8492(15) -0.2923(13) 0.3895(8) 0.050(4) Uani 1 1 d . . . . .
HM H 0.8848 -0.3524 0.4039 0.060 Uiso 1 1 calc R . . . .
C31 C 0.7484(15) -0.2920(14) 0.3689(10) 0.060(5) Uani 1 1 d . . . . .
HN H 0.7161 -0.3493 0.3699 0.072 Uiso 1 1 calc R . . . .
C32 C 0.6981(17) -0.2023(17) 0.3469(9) 0.065(6) Uani 1 1 d . . . . .
HO H 0.6332 -0.1991 0.3298 0.078 Uiso 1 1 calc R . . . .
Cu3 Cu 0.94418(15) 0.21944(13) 0.58854(8) 0.0329(4) Uani 1 1 d . . . . .
N5 N 0.7858(10) 0.2317(9) 0.5694(6) 0.036(3) Uani 1 1 d . . . . .
N6 N 0.6809(11) 0.1930(9) 0.4088(6) 0.043(3) Uani 1 1 d . . . . .
N7 N 0.6515(11) 0.0433(10) 0.3553(6) 0.042(3) Uani 1 1 d . . . . .
N8 N 0.9000(10) -0.2125(8) 0.3903(5) 0.033(3) Uani 1 1 d . . . . .
O41 O 0.5850(15) 0.3378(11) 0.4138(7) 0.084(5) Uani 1 1 d . U . . .
O42 O 0.6857(15) -0.0037(13) 0.2695(6) 0.088(6) Uani 1 1 d . U . . .
O47 O 0.8930(10) 0.1366(10) 0.6630(6) 0.059(3) Uani 1 1 d . U . . .
HP H 0.9236 0.1484 0.6932 0.089 Uiso 1 1 d GR . . . .
HQ H 0.9164 0.0733 0.6641 0.089 Uiso 1 1 d GR . . . .
O48 O 0.9821(8) 0.3179(7) 0.5174(4) 0.038(2) Uani 1 1 d . U . . .
HR H 0.9411 0.3721 0.5183 0.056 Uiso 1 1 d GR . . . .
HS H 0.9642 0.2999 0.4872 0.056 Uiso 1 1 d GR . . . .
O49 O 0.9798(10) 0.0868(8) 0.5436(5) 0.047(3) Uani 1 1 d . U . . .
HT H 0.9194 0.0747 0.5317 0.071 Uiso 1 1 d GR . . . .
HU H 0.9963 0.0344 0.5683 0.071 Uiso 1 1 d GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.022(7) 0.022(7) 0.045(8) 0.002(6) -0.002(6) -0.004(5)
C2 0.035(8) 0.041(9) 0.032(8) -0.005(7) 0.004(6) 0.009(7)
C3 0.017(6) 0.020(7) 0.047(8) -0.002(6) 0.006(6) -0.003(5)
C4 0.027(8) 0.037(9) 0.052(10) -0.014(7) 0.000(7) -0.007(7)
C5 0.017(7) 0.038(8) 0.038(8) -0.006(6) -0.004(6) -0.009(6)
C6 0.029(8) 0.038(9) 0.044(9) 0.003(7) 0.004(7) 0.009(7)
C7 0.028(8) 0.052(10) 0.037(8) 0.000(7) 0.002(6) 0.014(7)
C8 0.020(7) 0.038(8) 0.035(8) -0.004(6) -0.016(6) 0.003(6)
C9 0.030(8) 0.025(7) 0.037(8) -0.001(6) -0.002(6) -0.003(6)
C10 0.022(7) 0.039(8) 0.031(7) 0.001(6) -0.004(6) -0.005(6)
C11 0.028(8) 0.039(9) 0.038(8) -0.007(7) -0.006(6) -0.002(6)
C12 0.051(10) 0.033(9) 0.040(9) 0.006(7) -0.012(7) -0.008(7)
C13 0.034(8) 0.021(7) 0.044(8) 0.000(6) -0.009(7) -0.014(6)
C14 0.035(9) 0.038(9) 0.048(9) -0.004(7) -0.012(7) -0.001(7)
C15 0.041(10) 0.035(9) 0.070(12) -0.006(8) 0.002(9) 0.004(7)
C16 0.050(11) 0.033(9) 0.074(13) -0.008(9) 0.007(9) 0.005(8)
Co1 0.0191(9) 0.0168(9) 0.0293(9) 0.0000(7) -0.0021(7) 0.0004(7)
Co2 0.0193(9) 0.0205(9) 0.0299(9) -0.0017(7) -0.0026(7) -0.0032(7)
Cu1 0.0191(8) 0.0300(9) 0.0342(9) 0.0057(7) -0.0019(7) -0.0002(7)
Cu2 0.075(2) 0.098(2) 0.0767(19) 0.0045(17) -0.0047(16) -0.0111(18)
Mo1 0.0157(5) 0.0227(6) 0.0296(6) 0.0004(5) -0.0032(4) -0.0007(4)
Mo2 0.0269(6) 0.0265(6) 0.0296(6) -0.0036(5) -0.0013(5) -0.0006(5)
Mo3 0.0367(7) 0.0267(7) 0.0359(7) -0.0054(5) -0.0089(5) -0.0020(5)
Mo4 0.0280(7) 0.0305(7) 0.0454(8) 0.0018(6) -0.0079(6) -0.0084(5)
Mo5 0.0199(6) 0.0360(7) 0.0350(7) 0.0031(5) -0.0027(5) -0.0049(5)
Mo6 0.0270(6) 0.0199(6) 0.0385(7) -0.0002(5) -0.0072(5) -0.0013(5)
Mo7 0.0265(6) 0.0252(6) 0.0314(6) 0.0019(5) -0.0057(5) -0.0007(5)
Mo8 0.0307(7) 0.0277(7) 0.0325(7) -0.0048(5) -0.0042(5) -0.0010(5)
Mo9 0.0287(6) 0.0199(6) 0.0337(6) -0.0043(5) -0.0016(5) -0.0011(5)
Mo10 0.0183(5) 0.0209(6) 0.0296(6) -0.0002(5) -0.0032(4) 0.0007(4)
N1 0.014(5) 0.043(7) 0.039(7) 0.003(6) -0.007(5) -0.002(5)
N2 0.021(6) 0.050(8) 0.031(6) -0.002(6) -0.007(5) 0.010(6)
N3 0.018(6) 0.030(6) 0.037(6) -0.003(5) -0.004(5) -0.002(5)
N4 0.015(6) 0.035(7) 0.067(9) 0.005(6) 0.005(6) -0.004(5)
O1 0.032(5) 0.034(5) 0.039(5) 0.003(4) -0.009(4) 0.000(4)
O50 0.050(6) 0.065(7) 0.056(6) -0.013(6) 0.013(5) -0.007(6)
O2 0.024(3) 0.029(3) 0.040(4) -0.002(3) -0.007(3) -0.002(3)
O3 0.027(3) 0.025(3) 0.037(3) -0.007(3) -0.005(3) 0.001(3)
O4 0.022(3) 0.027(3) 0.034(3) -0.001(3) -0.003(2) -0.002(2)
O5 0.040(5) 0.029(5) 0.040(5) 0.003(4) -0.002(4) -0.009(4)
O6 0.039(5) 0.044(5) 0.040(5) -0.009(4) 0.002(4) -0.005(4)
O7 0.025(3) 0.034(3) 0.037(3) -0.002(3) -0.009(3) -0.001(3)
O8 0.024(3) 0.023(3) 0.038(3) -0.007(3) -0.005(3) 0.000(3)
O9 0.040(5) 0.032(5) 0.053(5) -0.013(4) -0.007(4) 0.000(4)
O10 0.044(5) 0.041(5) 0.049(5) -0.009(4) -0.018(4) -0.001(4)
O11 0.033(3) 0.030(3) 0.047(4) -0.002(3) -0.009(3) -0.003(3)
O12 0.025(3) 0.031(3) 0.037(3) -0.001(3) -0.007(3) -0.002(3)
O13 0.038(5) 0.045(6) 0.060(6) -0.004(5) -0.015(5) -0.004(5)
O14 0.042(5) 0.045(5) 0.062(6) 0.003(5) -0.005(5) -0.017(5)
O15 0.023(3) 0.027(3) 0.039(3) -0.002(3) -0.006(3) -0.004(3)
O16 0.027(3) 0.030(3) 0.046(4) 0.001(3) -0.003(3) -0.008(3)
O17 0.028(4) 0.043(5) 0.053(5) 0.012(4) -0.009(4) -0.007(4)
O18 0.023(5) 0.049(5) 0.048(5) -0.006(5) 0.004(4) 0.003(4)
O19 0.022(3) 0.026(3) 0.035(3) -0.001(3) -0.002(3) -0.001(3)
O20 0.023(3) 0.023(3) 0.035(3) -0.003(3) -0.004(3) -0.004(2)
O21 0.045(5) 0.030(5) 0.047(5) -0.013(4) -0.015(4) 0.013(4)
O22 0.041(5) 0.022(4) 0.054(5) 0.001(4) -0.008(4) -0.008(4)
O23 0.023(3) 0.025(3) 0.036(3) -0.001(3) -0.001(3) -0.003(3)
O24 0.031(3) 0.026(3) 0.038(3) 0.000(3) -0.004(3) 0.001(3)
O25 0.036(5) 0.036(5) 0.045(5) 0.010(4) 0.001(4) -0.004(4)
O26 0.030(5) 0.037(5) 0.044(5) 0.000(4) -0.011(4) -0.003(4)
O27 0.030(3) 0.032(3) 0.035(3) 0.002(3) -0.001(3) -0.002(3)
O28 0.024(3) 0.025(3) 0.032(3) -0.001(3) -0.001(3) 0.001(3)
O29 0.022(3) 0.023(3) 0.034(3) 0.001(3) -0.003(3) -0.004(3)
O30 0.045(5) 0.043(5) 0.040(5) -0.005(4) -0.005(4) -0.002(4)
O31 0.045(5) 0.039(5) 0.039(5) -0.004(4) -0.010(4) -0.005(4)
O32 0.029(3) 0.027(3) 0.037(3) -0.001(3) -0.001(3) -0.001(3)
O33 0.038(5) 0.030(5) 0.042(5) -0.001(4) 0.001(4) -0.005(4)
O34 0.034(4) 0.034(4) 0.040(4) -0.006(4) -0.002(4) -0.005(4)
O35 0.025(3) 0.024(3) 0.036(3) -0.001(3) -0.003(3) 0.001(3)
O36 0.022(3) 0.022(3) 0.034(3) -0.004(2) -0.002(2) -0.005(2)
O37 0.024(4) 0.038(5) 0.042(5) -0.003(4) -0.005(4) -0.003(4)
O38 0.026(3) 0.023(3) 0.034(4) 0.001(3) -0.001(3) 0.001(3)
O39 0.031(6) 0.047(7) 0.066(8) 0.018(6) 0.004(6) 0.003(5)
O40 0.044(6) 0.090(8) 0.043(6) 0.005(6) 0.001(5) 0.006(6)
O43 0.059(7) 0.080(8) 0.080(7) 0.009(7) -0.005(6) -0.010(6)
O44 0.092(4) 0.093(4) 0.092(4) -0.016(2) -0.009(2) -0.007(2)
O45 0.084(9) 0.093(9) 0.090(8) -0.016(8) -0.001(7) -0.013(8)
O46 0.106(9) 0.092(9) 0.096(9) 0.001(8) 0.011(8) -0.008(8)
C17 0.037(9) 0.064(12) 0.056(11) -0.023(9) -0.003(8) -0.013(9)
C18 0.045(10) 0.050(10) 0.039(9) -0.005(8) -0.010(7) -0.007(8)
C19 0.039(10) 0.073(14) 0.077(14) -0.031(11) -0.005(9) -0.017(10)
C20 0.029(10) 0.091(17) 0.103(17) -0.053(14) -0.020(10) 0.006(10)
C21 0.026(8) 0.039(9) 0.078(12) -0.011(8) -0.020(8) -0.020(7)
C22 0.047(11) 0.053(12) 0.068(13) 0.011(10) -0.017(9) -0.005(9)
C23 0.022(7) 0.030(8) 0.064(11) 0.006(7) 0.000(7) 0.001(6)
C24 0.045(10) 0.052(11) 0.044(10) 0.005(8) 0.003(8) 0.003(8)
C25 0.049(10) 0.039(10) 0.049(10) 0.004(8) -0.008(8) -0.005(8)
C26 0.027(8) 0.043(10) 0.055(10) -0.003(8) 0.008(7) -0.012(7)
C27 0.061(12) 0.035(9) 0.057(11) -0.010(8) -0.016(9) 0.009(8)
C28 0.046(10) 0.064(12) 0.029(8) -0.002(8) -0.009(7) 0.001(9)
C29 0.027(8) 0.038(9) 0.055(10) 0.003(7) -0.016(7) 0.007(7)
C30 0.043(10) 0.040(10) 0.063(11) -0.009(8) -0.002(8) 0.003(8)
C31 0.032(9) 0.046(11) 0.106(17) -0.021(11) -0.015(10) -0.009(8)
C32 0.046(12) 0.076(15) 0.078(14) -0.026(12) -0.018(10) 0.000(11)
Cu3 0.0276(9) 0.0258(9) 0.0431(10) -0.0016(8) -0.0027(8) -0.0039(7)
N5 0.018(6) 0.030(7) 0.063(9) -0.012(6) -0.009(6) -0.005(5)
N6 0.038(8) 0.025(7) 0.064(9) 0.000(6) -0.014(7) -0.001(6)
N7 0.042(8) 0.039(8) 0.045(8) -0.001(6) -0.010(6) -0.007(6)
N8 0.035(7) 0.022(6) 0.037(7) -0.005(5) 0.008(5) -0.001(5)
O41 0.099(13) 0.059(10) 0.086(11) -0.004(8) -0.028(9) 0.030(9)
O42 0.110(13) 0.100(13) 0.047(8) -0.018(8) -0.024(8) 0.051(10)
O47 0.049(6) 0.051(7) 0.062(7) 0.009(6) 0.008(6) 0.001(5)
O48 0.033(5) 0.027(5) 0.045(5) 0.007(4) -0.003(4) 0.001(4)
O49 0.046(6) 0.030(5) 0.064(7) -0.001(5) -0.004(5) -0.013(5)
_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
C1 C5 1.365(18) . ?
C1 N1 1.360(18) . ?
C2 C3 1.34(2) . ?
C2 N1 1.371(19) . ?
C3 C4 1.37(2) . ?
C4 C5 1.39(2) . ?
C5 C6 1.54(2) . ?
C6 N2 1.287(19) . ?
C6 O40 1.235(19) . ?
C7 C8 1.49(2) 2_567 ?
C7 N2 1.489(18) . ?
C8 C7 1.49(2) 2_567 ?
C8 N2 1.484(17) . ?
C9 C11 1.39(2) . ?
C9 N3 1.351(18) . ?
C10 C13 1.404(19) . ?
C10 N3 1.362(18) . ?
C11 C12 1.38(2) . ?
C12 C13 1.38(2) . ?
C13 C14 1.53(2) . ?
C14 N4 1.34(2) . ?
C14 O39 1.230(19) . ?
C15 C16 1.45(2) . ?
C15 N4 1.44(2) . ?
C16 N4 1.48(2) 2_757 ?
Co1 Co2 2.790(3) . ?
Co1 Mo1 2.983(2) . ?
Co1 Mo5 3.051(2) . ?
Co1 O19 1.882(9) . ?
Co1 O20 1.874(10) . ?
Co1 O23 1.925(9) . ?
Co1 O28 1.930(10) . ?
Co1 O29 1.940(9) . ?
Co1 O36 1.888(9) . ?
Co2 Mo6 3.037(2) . ?
Co2 Mo10 2.974(2) . ?
Co2 O4 1.880(9) . ?
Co2 O8 1.941(9) . ?
Co2 O12 1.938(9) . ?
Co2 O15 1.907(9) . ?
Co2 O19 1.895(10) . ?
Co2 O20 1.888(9) . ?
Cu1 N1 2.017(11) . ?
Cu1 N3 1.999(11) . ?
Cu1 O50 2.325(13) . ?
Cu1 O2 1.988(10) . ?
Cu1 O38 1.986(9) . ?
Cu2 O40 2.028(14) . ?
Cu2 O43 1.951(15) . ?
Cu2 O44 2.225(18) . ?
Cu2 O45 1.972(17) . ?
Cu2 O46 1.963(18) . ?
Mo1 O1 1.693(10) . ?
Mo1 O2 1.768(10) . ?
Mo1 O3 1.858(9) . ?
Mo1 O4 2.280(9) . ?
Mo1 O20 2.195(9) . ?
Mo1 O36 2.034(9) . ?
Mo2 O3 1.974(9) . ?
Mo2 O4 2.300(10) . ?
Mo2 O5 1.718(10) . ?
Mo2 O6 1.673(11) . ?
Mo2 O7 1.899(9) . ?
Mo2 O8 2.265(9) . ?
Mo3 O7 1.940(10) . ?
Mo3 O8 2.318(9) . ?
Mo3 O9 1.718(11) . ?
Mo3 O10 1.704(11) . ?
Mo3 O11 1.937(10) . ?
Mo3 O12 2.297(10) . ?
Mo4 O11 1.926(11) . ?
Mo4 O12 2.257(10) . ?
Mo4 O13 1.683(11) . ?
Mo4 O14 1.725(11) . ?
Mo4 O15 2.386(9) . ?
Mo4 O16 1.954(11) . ?
Mo5 O15 2.287(10) . ?
Mo5 O16 1.898(10) . ?
Mo5 O17 1.687(10) . ?
Mo5 O18 1.735(11) . ?
Mo5 O19 2.409(9) . ?
Mo5 O23 1.977(9) . ?
Mo6 O15 1.989(9) . ?
Mo6 O20 2.413(9) . ?
Mo6 O21 1.718(11) . ?
Mo6 O22 1.706(10) . ?
Mo6 O23 2.271(10) . ?
Mo6 O24 1.867(10) . ?
Mo7 O23 2.319(10) . ?
Mo7 O24 1.953(10) . ?
Mo7 O25 1.708(10) . ?
Mo7 O26 1.712(10) . ?
Mo7 O27 1.951(10) . ?
Mo7 O29 2.286(9) . ?
Mo8 O27 1.935(10) . ?
Mo8 O28 2.287(9) . ?
Mo8 O29 2.278(10) . ?
Mo8 O30 1.714(11) . ?
Mo8 O31 1.712(11) . ?
Mo8 O32 1.946(9) . ?
Mo9 O28 2.237(9) . ?
Mo9 O32 1.897(10) . ?
Mo9 O33 1.702(11) . ?
Mo9 O34 1.704(10) . ?
Mo9 O35 1.998(10) . ?
Mo9 O36 2.288(9) . ?
Mo10 O4 2.009(10) . ?
Mo10 O19 2.152(9) . ?
Mo10 O35 1.850(10) . ?
Mo10 O36 2.278(9) . ?
Mo10 O37 1.739(10) . ?
Mo10 O38 1.736(9) . ?
N4 C16 1.48(2) 2_757 ?
C17 C19 1.36(2) . ?
C17 N5 1.32(2) . ?
C18 C21 1.35(2) . ?
C18 N5 1.35(2) . ?
C19 C20 1.35(3) . ?
C20 C21 1.33(3) . ?
C21 C22 1.52(3) . ?
C22 N6 1.34(3) . ?
C22 O41 1.27(2) . ?
C23 C24 1.42(2) . ?
C23 N6 1.46(2) . ?
C24 N7 1.48(2) . ?
C25 C26 1.51(2) . ?
C25 N6 1.49(2) . ?
C26 N7 1.44(2) . ?
C27 C28 1.48(2) . ?
C27 N7 1.31(2) . ?
C27 O42 1.26(2) . ?
C28 C29 1.41(2) . ?
C28 C32 1.37(3) . ?
C29 N8 1.356(19) . ?
C30 C31 1.38(2) . ?
C30 N8 1.35(2) . ?
C31 C32 1.38(3) . ?
Cu3 N5 2.019(12) . ?
Cu3 N8 2.012(13) 2_756 ?
Cu3 O47 1.977(12) . ?
Cu3 O48 1.994(10) . ?
Cu3 O49 2.316(12) . ?
N8 Cu3 2.012(13) 2_756 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C5 120.5(13) . . ?
C3 C2 N1 121.7(14) . . ?
C2 C3 C4 120.6(14) . . ?
C3 C4 C5 118.2(14) . . ?
C1 C5 C4 120.3(14) . . ?
C1 C5 C6 116.9(13) . . ?
C4 C5 C6 122.6(13) . . ?
N2 C6 C5 120.7(14) . . ?
O40 C6 C5 116.3(14) . . ?
O40 C6 N2 122.8(14) . . ?
N2 C7 C8 109.6(13) . 2_567 ?
N2 C8 C7 110.6(11) . 2_567 ?
N3 C9 C11 122.4(14) . . ?
N3 C10 C13 121.1(14) . . ?
C12 C11 C9 119.4(15) . . ?
C13 C12 C11 118.7(15) . . ?
C10 C13 C14 115.4(14) . . ?
C12 C13 C10 120.0(15) . . ?
C12 C13 C14 124.2(14) . . ?
N4 C14 C13 119.6(14) . . ?
O39 C14 C13 117.5(14) . . ?
O39 C14 N4 122.8(15) . . ?
N4 C15 C16 112.5(16) . . ?
C15 C16 N4 109.8(15) . 2_757 ?
Co2 Co1 Mo1 67.17(6) . . ?
Co2 Co1 Mo5 67.80(6) . . ?
Mo1 Co1 Mo5 134.96(7) . . ?
O19 Co1 Co2 42.5(3) . . ?
O19 Co1 Mo1 93.1(3) . . ?
O19 Co1 Mo5 52.1(3) . . ?
O19 Co1 O23 89.3(4) . . ?
O19 Co1 O28 94.3(4) . . ?
O19 Co1 O29 175.7(4) . . ?
O19 Co1 O36 84.9(4) . . ?
O20 Co1 Co2 42.3(3) . . ?
O20 Co1 Mo1 47.2(3) . . ?
O20 Co1 Mo5 96.3(3) . . ?
O20 Co1 O19 84.7(4) . . ?
O20 Co1 O23 88.6(4) . . ?
O20 Co1 O28 173.9(4) . . ?
O20 Co1 O29 97.2(4) . . ?
O20 Co1 O36 87.6(4) . . ?
O23 Co1 Co2 85.8(3) . . ?
O23 Co1 Mo1 135.1(3) . . ?
O23 Co1 Mo5 39.2(3) . . ?
O23 Co1 O28 97.4(4) . . ?
O23 Co1 O29 87.0(4) . . ?
O28 Co1 Co2 136.8(3) . . ?
O28 Co1 Mo1 127.0(3) . . ?
O28 Co1 Mo5 87.8(3) . . ?
O28 Co1 O29 84.2(4) . . ?
O29 Co1 Co2 139.0(3) . . ?
O29 Co1 Mo1 91.0(3) . . ?
O29 Co1 Mo5 123.7(3) . . ?
O36 Co1 Co2 87.8(3) . . ?
O36 Co1 Mo1 42.3(3) . . ?
O36 Co1 Mo5 136.0(3) . . ?
O36 Co1 O23 173.4(4) . . ?
O36 Co1 O28 86.3(4) . . ?
O36 Co1 O29 98.9(4) . . ?
Co1 Co2 Mo6 68.49(6) . . ?
Co1 Co2 Mo10 67.36(6) . . ?
Mo10 Co2 Mo6 135.80(7) . . ?
O4 Co2 Co1 87.6(3) . . ?
O4 Co2 Mo6 138.0(3) . . ?
O4 Co2 Mo10 41.8(3) . . ?
O4 Co2 O8 87.2(4) . . ?
O4 Co2 O12 95.5(4) . . ?
O4 Co2 O15 175.1(4) . . ?
O4 Co2 O19 85.9(4) . . ?
O4 Co2 O20 86.4(4) . . ?
O8 Co2 Co1 137.6(3) . . ?
O8 Co2 Mo6 88.3(3) . . ?
O8 Co2 Mo10 127.1(3) . . ?
O12 Co2 Co1 136.9(3) . . ?
O12 Co2 Mo6 125.7(3) . . ?
O12 Co2 Mo10 86.9(3) . . ?
O12 Co2 O8 85.5(4) . . ?
O15 Co2 Co1 87.5(3) . . ?
O15 Co2 Mo6 39.8(3) . . ?
O15 Co2 Mo10 135.0(3) . . ?
O15 Co2 O8 96.8(4) . . ?
O15 Co2 O12 87.6(4) . . ?
O19 Co2 Co1 42.2(3) . . ?
O19 Co2 Mo6 96.9(3) . . ?
O19 Co2 Mo10 46.2(3) . . ?
O19 Co2 O8 173.1(4) . . ?
O19 Co2 O12 95.1(4) . . ?
O19 Co2 O15 90.0(4) . . ?
O20 Co2 Co1 41.9(3) . . ?
O20 Co2 Mo6 52.6(3) . . ?
O20 Co2 Mo10 93.8(3) . . ?
O20 Co2 O8 95.7(4) . . ?
O20 Co2 O12 177.8(4) . . ?
O20 Co2 O15 90.4(4) . . ?
O20 Co2 O19 84.0(4) . . ?
N1 Cu1 O50 87.5(5) . . ?
N3 Cu1 N1 92.7(5) . . ?
N3 Cu1 O50 95.4(5) . . ?
O2 Cu1 N1 91.5(4) . . ?
O2 Cu1 N3 169.4(5) . . ?
O2 Cu1 O50 94.5(4) . . ?
O38 Cu1 N1 174.6(5) . . ?
O38 Cu1 N3 88.3(4) . . ?
O38 Cu1 O50 87.0(4) . . ?
O38 Cu1 O2 88.4(4) . . ?
O40 Cu2 O44 101.1(6) . . ?
O43 Cu2 O40 86.3(6) . . ?
O43 Cu2 O44 91.1(7) . . ?
O43 Cu2 O45 91.9(7) . . ?
O43 Cu2 O46 175.0(8) . . ?
O45 Cu2 O40 167.4(7) . . ?
O45 Cu2 O44 91.4(7) . . ?
O46 Cu2 O40 94.9(7) . . ?
O46 Cu2 O44 93.4(8) . . ?
O46 Cu2 O45 85.8(8) . . ?
O1 Mo1 Co1 90.3(4) . . ?
O1 Mo1 O2 105.2(5) . . ?
O1 Mo1 O3 105.6(5) . . ?
O1 Mo1 O4 163.3(4) . . ?
O1 Mo1 O20 92.9(4) . . ?
O1 Mo1 O36 100.7(4) . . ?
O2 Mo1 Co1 129.1(3) . . ?
O2 Mo1 O3 98.6(4) . . ?
O2 Mo1 O4 91.1(4) . . ?
O2 Mo1 O20 159.2(4) . . ?
O2 Mo1 O36 90.5(4) . . ?
O3 Mo1 Co1 123.8(3) . . ?
O3 Mo1 O4 74.7(4) . . ?
O3 Mo1 O20 86.0(4) . . ?
O3 Mo1 O36 148.7(4) . . ?
O4 Mo1 Co1 76.3(2) . . ?
O20 Mo1 Co1 38.8(2) . . ?
O20 Mo1 O4 70.4(3) . . ?
O36 Mo1 Co1 38.7(2) . . ?
O36 Mo1 O4 75.2(4) . . ?
O36 Mo1 O20 75.9(4) . . ?
O3 Mo2 O4 72.2(4) . . ?
O3 Mo2 O8 79.1(4) . . ?
O5 Mo2 O3 98.7(4) . . ?
O5 Mo2 O4 89.0(4) . . ?
O5 Mo2 O7 101.8(5) . . ?
O5 Mo2 O8 159.2(4) . . ?
O6 Mo2 O3 95.7(5) . . ?
O6 Mo2 O4 162.5(4) . . ?
O6 Mo2 O5 105.6(5) . . ?
O6 Mo2 O7 101.1(5) . . ?
O6 Mo2 O8 95.2(4) . . ?
O7 Mo2 O3 148.8(4) . . ?
O7 Mo2 O4 84.8(4) . . ?
O7 Mo2 O8 73.3(4) . . ?
O8 Mo2 O4 70.5(3) . . ?
O7 Mo3 O8 71.4(4) . . ?
O7 Mo3 O12 80.8(4) . . ?
O9 Mo3 O7 101.7(5) . . ?
O9 Mo3 O8 93.1(4) . . ?
O9 Mo3 O11 98.3(5) . . ?
O9 Mo3 O12 160.9(4) . . ?
O10 Mo3 O7 96.0(5) . . ?
O10 Mo3 O8 159.6(4) . . ?
O10 Mo3 O9 105.4(5) . . ?
O10 Mo3 O11 102.3(5) . . ?
O10 Mo3 O12 93.1(5) . . ?
O11 Mo3 O7 148.1(4) . . ?
O11 Mo3 O8 83.0(4) . . ?
O11 Mo3 O12 72.5(4) . . ?
O12 Mo3 O8 69.5(3) . . ?
O11 Mo4 O12 73.6(4) . . ?
O11 Mo4 O15 83.5(4) . . ?
O11 Mo4 O16 148.7(4) . . ?
O12 Mo4 O15 69.9(3) . . ?
O13 Mo4 O11 100.4(5) . . ?
O13 Mo4 O12 94.3(5) . . ?
O13 Mo4 O14 106.3(6) . . ?
O13 Mo4 O15 162.1(5) . . ?
O13 Mo4 O16 97.6(5) . . ?
O14 Mo4 O11 97.3(5) . . ?
O14 Mo4 O12 158.8(5) . . ?
O14 Mo4 O15 90.4(5) . . ?
O14 Mo4 O16 102.0(5) . . ?
O16 Mo4 O12 79.8(4) . . ?
O16 Mo4 O15 72.0(4) . . ?
O15 Mo5 Co1 75.1(2) . . ?
O15 Mo5 O19 69.8(3) . . ?
O16 Mo5 Co1 119.9(3) . . ?
O16 Mo5 O15 75.3(4) . . ?
O16 Mo5 O19 82.7(4) . . ?
O16 Mo5 O23 146.2(4) . . ?
O17 Mo5 Co1 134.1(4) . . ?
O17 Mo5 O15 98.1(5) . . ?
O17 Mo5 O16 101.0(5) . . ?
O17 Mo5 O18 105.6(6) . . ?
O17 Mo5 O19 166.3(4) . . ?
O17 Mo5 O23 96.3(4) . . ?
O18 Mo5 Co1 86.2(4) . . ?
O18 Mo5 O15 156.2(4) . . ?
O18 Mo5 O16 102.4(5) . . ?
O18 Mo5 O19 86.3(4) . . ?
O18 Mo5 O23 100.7(5) . . ?
O19 Mo5 Co1 38.1(2) . . ?
O23 Mo5 Co1 37.9(3) . . ?
O23 Mo5 O15 73.6(4) . . ?
O23 Mo5 O19 74.4(3) . . ?
O15 Mo6 Co2 37.8(3) . . ?
O15 Mo6 O20 74.7(3) . . ?
O15 Mo6 O23 73.7(4) . . ?
O20 Mo6 Co2 38.4(2) . . ?
O21 Mo6 Co2 86.0(3) . . ?
O21 Mo6 O15 100.5(5) . . ?
O21 Mo6 O20 85.9(4) . . ?
O21 Mo6 O23 154.8(4) . . ?
O21 Mo6 O24 104.3(5) . . ?
O22 Mo6 Co2 132.1(4) . . ?
O22 Mo6 O15 94.4(5) . . ?
O22 Mo6 O20 166.0(4) . . ?
O22 Mo6 O21 105.1(5) . . ?
O22 Mo6 O23 99.8(4) . . ?
O22 Mo6 O24 100.3(5) . . ?
O23 Mo6 Co2 74.5(2) . . ?
O23 Mo6 O20 68.9(3) . . ?
O24 Mo6 Co2 122.3(3) . . ?
O24 Mo6 O15 146.6(4) . . ?
O24 Mo6 O20 85.0(4) . . ?
O24 Mo6 O23 74.3(4) . . ?
O24 Mo7 O23 71.7(4) . . ?
O24 Mo7 O29 81.9(4) . . ?
O25 Mo7 O23 89.8(4) . . ?
O25 Mo7 O24 101.2(5) . . ?
O25 Mo7 O26 105.4(5) . . ?
O25 Mo7 O27 98.0(5) . . ?
O25 Mo7 O29 158.2(4) . . ?
O26 Mo7 O23 162.9(4) . . ?
O26 Mo7 O24 97.3(5) . . ?
O26 Mo7 O27 100.4(5) . . ?
O26 Mo7 O29 95.4(4) . . ?
O27 Mo7 O23 84.8(4) . . ?
O27 Mo7 O24 149.3(4) . . ?
O27 Mo7 O29 71.6(4) . . ?
O29 Mo7 O23 70.5(3) . . ?
O27 Mo8 O28 82.0(4) . . ?
O27 Mo8 O29 72.1(4) . . ?
O27 Mo8 O32 146.9(4) . . ?
O29 Mo8 O28 69.3(3) . . ?
O30 Mo8 O27 97.5(5) . . ?
O30 Mo8 O28 91.3(4) . . ?
O30 Mo8 O29 158.8(4) . . ?
O30 Mo8 O32 101.7(5) . . ?
O31 Mo8 O27 102.2(5) . . ?
O31 Mo8 O28 162.6(4) . . ?
O31 Mo8 O29 95.7(4) . . ?
O31 Mo8 O30 104.7(5) . . ?
O31 Mo8 O32 98.7(5) . . ?
O32 Mo8 O28 70.9(4) . . ?
O32 Mo8 O29 80.5(4) . . ?
O28 Mo9 O36 70.5(3) . . ?
O32 Mo9 O28 72.9(4) . . ?
O32 Mo9 O35 149.6(4) . . ?
O32 Mo9 O36 85.1(4) . . ?
O33 Mo9 O28 95.5(4) . . ?
O33 Mo9 O32 101.9(5) . . ?
O33 Mo9 O34 104.0(5) . . ?
O33 Mo9 O35 95.2(5) . . ?
O33 Mo9 O36 162.0(4) . . ?
O34 Mo9 O28 160.4(4) . . ?
O34 Mo9 O32 100.3(5) . . ?
O34 Mo9 O35 99.8(4) . . ?
O34 Mo9 O36 90.8(4) . . ?
O35 Mo9 O28 80.6(4) . . ?
O35 Mo9 O36 72.0(4) . . ?
O4 Mo10 Co2 38.6(3) . . ?
O4 Mo10 O19 76.3(4) . . ?
O4 Mo10 O36 75.7(4) . . ?
O19 Mo10 Co2 39.4(3) . . ?
O19 Mo10 O36 70.1(3) . . ?
O35 Mo10 Co2 125.9(3) . . ?
O35 Mo10 O4 149.7(4) . . ?
O35 Mo10 O19 87.4(4) . . ?
O35 Mo10 O36 74.8(4) . . ?
O36 Mo10 Co2 76.8(2) . . ?
O37 Mo10 Co2 90.5(3) . . ?
O37 Mo10 O4 102.9(4) . . ?
O37 Mo10 O19 91.4(4) . . ?
O37 Mo10 O35 102.8(5) . . ?
O37 Mo10 O36 161.3(4) . . ?
O38 Mo10 Co2 125.9(3) . . ?
O38 Mo10 O4 87.4(4) . . ?
O38 Mo10 O19 158.9(4) . . ?
O38 Mo10 O35 100.9(4) . . ?
O38 Mo10 O36 93.2(4) . . ?
O38 Mo10 O37 105.5(5) . . ?
C1 N1 C2 118.7(12) . . ?
C1 N1 Cu1 121.7(10) . . ?
C2 N1 Cu1 119.4(10) . . ?
C6 N2 C7 120.0(13) . . ?
C6 N2 C8 127.4(12) . . ?
C8 N2 C7 112.4(11) . . ?
C9 N3 C10 118.2(12) . . ?
C9 N3 Cu1 123.2(10) . . ?
C10 N3 Cu1 118.1(9) . . ?
C14 N4 C15 121.0(13) . . ?
C14 N4 C16 124.4(14) . 2_757 ?
C15 N4 C16 114.2(13) . 2_757 ?
Mo1 O2 Cu1 136.6(5) . . ?
Mo1 O3 Mo2 117.1(5) . . ?
Co2 O4 Mo1 100.0(4) . . ?
Co2 O4 Mo2 101.4(4) . . ?
Co2 O4 Mo10 99.7(4) . . ?
Mo1 O4 Mo2 91.0(3) . . ?
Mo10 O4 Mo1 102.5(4) . . ?
Mo10 O4 Mo2 152.5(5) . . ?
Mo2 O7 Mo3 118.5(5) . . ?
Co2 O8 Mo2 100.8(4) . . ?
Co2 O8 Mo3 102.1(4) . . ?
Mo2 O8 Mo3 92.1(3) . . ?
Mo4 O11 Mo3 116.2(5) . . ?
Co2 O12 Mo3 102.9(4) . . ?
Co2 O12 Mo4 103.0(4) . . ?
Mo4 O12 Mo3 92.1(4) . . ?
Co2 O15 Mo4 99.4(4) . . ?
Co2 O15 Mo5 101.9(4) . . ?
Co2 O15 Mo6 102.4(4) . . ?
Mo5 O15 Mo4 89.5(3) . . ?
Mo6 O15 Mo4 152.6(5) . . ?
Mo6 O15 Mo5 102.0(4) . . ?
Mo5 O16 Mo4 117.2(5) . . ?
Co1 O19 Co2 95.3(4) . . ?
Co1 O19 Mo5 89.8(4) . . ?
Co1 O19 Mo10 104.8(4) . . ?
Co2 O19 Mo5 98.0(4) . . ?
Co2 O19 Mo10 94.4(4) . . ?
Mo10 O19 Mo5 159.9(5) . . ?
Co1 O20 Co2 95.7(4) . . ?
Co1 O20 Mo1 94.0(4) . . ?
Co1 O20 Mo6 99.3(4) . . ?
Co2 O20 Mo1 102.8(4) . . ?
Co2 O20 Mo6 89.0(3) . . ?
Mo1 O20 Mo6 161.3(4) . . ?
Co1 O23 Mo5 102.9(4) . . ?
Co1 O23 Mo6 102.8(4) . . ?
Co1 O23 Mo7 100.9(4) . . ?
Mo5 O23 Mo6 102.9(4) . . ?
Mo5 O23 Mo7 148.9(5) . . ?
Mo6 O23 Mo7 91.0(3) . . ?
Mo6 O24 Mo7 117.9(5) . . ?
Mo8 O27 Mo7 117.8(5) . . ?
Co1 O28 Mo8 103.2(4) . . ?
Co1 O28 Mo9 101.8(4) . . ?
Mo9 O28 Mo8 92.9(3) . . ?
Co1 O29 Mo7 101.6(4) . . ?
Co1 O29 Mo8 103.3(4) . . ?
Mo8 O29 Mo7 93.6(3) . . ?
Mo9 O32 Mo8 117.2(5) . . ?
Mo10 O35 Mo9 117.7(5) . . ?
Co1 O36 Mo1 99.0(4) . . ?
Co1 O36 Mo9 101.3(4) . . ?
Co1 O36 Mo10 100.0(4) . . ?
Mo1 O36 Mo9 152.9(4) . . ?
Mo1 O36 Mo10 101.8(4) . . ?
Mo10 O36 Mo9 92.3(3) . . ?
Mo10 O38 Cu1 142.6(5) . . ?
C6 O40 Cu2 135.3(14) . . ?
N5 C17 C19 122.7(18) . . ?
N5 C18 C21 121.5(17) . . ?
C20 C19 C17 118.7(19) . . ?
C21 C20 C19 119.1(18) . . ?
C18 C21 C22 117.6(17) . . ?
C20 C21 C18 120.6(18) . . ?
C20 C21 C22 121.3(16) . . ?
N6 C22 C21 120.7(16) . . ?
O41 C22 C21 120(2) . . ?
O41 C22 N6 119.7(19) . . ?
C24 C23 N6 113.0(13) . . ?
C23 C24 N7 108.5(14) . . ?
N6 C25 C26 108.2(14) . . ?
N7 C26 C25 109.6(13) . . ?
N7 C27 C28 120.3(16) . . ?
O42 C27 C28 117.4(16) . . ?
O42 C27 N7 122.2(16) . . ?
C29 C28 C27 119.6(17) . . ?
C32 C28 C27 122.7(17) . . ?
C32 C28 C29 117.0(18) . . ?
N8 C29 C28 122.6(16) . . ?
N8 C30 C31 125.2(17) . . ?
C32 C31 C30 116.3(17) . . ?
C28 C32 C31 122.0(18) . . ?
N5 Cu3 O49 88.6(5) . . ?
N8 Cu3 N5 177.2(5) 2_756 . ?
N8 Cu3 O49 94.2(5) 2_756 . ?
O47 Cu3 N5 87.6(5) . . ?
O47 Cu3 N8 92.1(5) . 2_756 ?
O47 Cu3 O48 172.0(5) . . ?
O47 Cu3 O49 91.9(5) . . ?
O48 Cu3 N5 89.0(5) . . ?
O48 Cu3 N8 90.9(4) . 2_756 ?
O48 Cu3 O49 95.2(4) . . ?
C17 N5 C18 117.2(14) . . ?
C17 N5 Cu3 121.3(12) . . ?
C18 N5 Cu3 121.4(11) . . ?
C22 N6 C23 121.7(14) . . ?
C22 N6 C25 124.5(15) . . ?
C23 N6 C25 113.4(13) . . ?
C26 N7 C24 114.8(14) . . ?
C27 N7 C24 120.7(15) . . ?
C27 N7 C26 124.3(15) . . ?
C29 N8 Cu3 120.5(10) . 2_756 ?
C30 N8 C29 116.6(14) . . ?
C30 N8 Cu3 122.6(11) . 2_756 ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.101 0.000 0.000 734.0 327.7 ?
2 0.444 0.938 0.407 7.2 0.0 ?
3 0.556 0.062 0.593 7.2 0.0 ?
_shelx_fab_file
;
-16 -4 1 2.6610 0.3899
-16 -4 2 7.4221 0.0676
-16 -3 1 -2.1078 0.0882
-16 -1 1 0.4008 -0.5180
-16 0 1 4.3820 -0.2132
-16 1 1 -0.2018 0.3880
-16 2 1 4.3751 0.7117
-15 -6 1 -2.7542 0.2169
-15 -6 2 -8.3353 0.2749
-15 -5 1 -0.5524 0.0689
-15 -5 2 -8.8395 0.2483
-15 -5 3 -5.5922 0.1350
-15 -5 4 1.5669 -0.2049
-15 -5 5 4.3742 -0.0866
-15 -4 1 -0.2605 0.1156
-15 -4 2 -5.6225 0.0921
-15 -4 3 -6.8273 0.1032
-15 -4 4 7.1211 -0.0000
-15 -4 5 7.1270 -0.1570
-15 -4 6 1.3806 -0.0324
-15 -3 1 0.0385 0.2287
-15 -3 2 -3.1682 0.1030
-15 -3 3 -0.3406 0.0313
-15 -3 4 -1.5431 -0.0226
-15 -3 5 5.7877 -0.0182
-15 -3 6 2.2880 -0.0467
-15 -3 7 -1.4128 0.0083
-15 -2 1 -2.0323 -0.3137
-15 -2 2 4.2804 0.2415
-15 -2 3 -3.9158 0.0840
-15 -2 4 -0.6048 -0.0760
-15 -2 5 -4.8434 -0.0977
-15 -1 1 -5.7280 -0.5030
-15 -1 2 -2.6281 -0.2792
-15 0 1 -5.3683 -0.2294
-15 0 2 -2.5199 -0.5713
-15 0 3 -6.3385 -0.3592
-15 1 1 -6.2540 0.3582
-15 1 2 -6.5762 -0.3924
-15 1 3 -1.3650 -0.6198
-15 2 1 -4.9183 0.6620
-15 2 2 -0.4076 0.2285
-15 2 3 -2.8378 -0.2495
-15 3 1 -9.6810 -0.4754
-15 3 2 0.4937 0.5288
-15 3 3 6.3659 0.3263
-15 4 1 -1.2737 -0.0570
-15 4 2 -0.4350 -0.2251
-15 4 3 -0.5236 0.3751
-15 5 1 3.7642 -0.2659
-15 5 2 -4.6195 0.1070
-15 5 3 2.6096 -0.0579
-14 -9 1 4.3941 -0.3750
-14 -8 1 4.7579 0.0276
-14 -8 2 6.6011 -0.4215
-14 -7 1 -1.7248 0.6552
-14 -7 2 3.9699 0.0001
-14 -7 3 9.0472 -0.3412
-14 -6 1 -2.4119 -0.2165
-14 -6 2 4.0962 0.5778
-14 -6 3 9.9559 0.0920
-14 -6 4 8.4868 -0.2501
-14 -5 1 -3.6423 -0.0989
-14 -5 2 3.4794 -0.2389
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15 0 7 3.1030 -0.0321
15 0 8 -7.4656 -0.0661
15 0 9 -14.6188 0.3065
15 1 0 -5.8524 0.1676
15 1 1 -3.7819 -0.3292
15 1 2 9.9662 -0.4852
15 1 3 6.8688 0.1714
15 1 4 -7.1329 0.0253
15 1 5 -7.8450 -0.3368
15 1 6 -3.2478 0.2411
15 1 7 12.0722 0.2382
15 1 8 8.9005 -0.0145
15 1 9 -1.7888 -0.0658
15 1 10 -5.3818 0.0755
15 2 0 -8.0329 0.4586
15 2 1 -1.2891 0.0165
15 2 2 0.6529 -0.3361
15 2 3 4.5129 -0.2582
15 2 4 7.3579 0.1328
15 2 5 0.9869 -0.0242
15 2 6 1.2695 -0.2014
15 2 7 0.7927 0.2077
15 2 8 6.8878 0.1519
15 2 9 7.9472 -0.1355
15 2 10 -2.8150 -0.0011
15 3 0 -2.3852 0.2845
15 3 1 -5.8221 0.3054
15 3 2 1.0598 -0.1148
15 3 3 2.3057 -0.1672
15 3 4 3.3638 0.0417
15 3 5 12.9187 0.1219
15 3 6 7.1427 -0.1196
15 3 7 -2.3727 -0.1260
15 3 8 -2.4320 0.0963
15 3 9 1.6933 0.1113
15 3 10 2.0588 -0.1314
15 4 0 -1.6640 -0.2260
15 4 1 -1.2599 0.2416
15 4 2 0.4013 0.3278
15 4 3 2.5067 -0.0613
15 4 4 2.3537 -0.0621
15 4 5 0.6900 0.0809
15 4 6 7.9534 0.0607
15 4 7 3.9517 -0.1173
15 4 8 -5.1001 -0.0386
15 4 9 -2.9796 -0.0828
15 4 10 -4.7368 0.0339
15 4 11 -5.2935 -0.0357
15 5 0 4.0164 -0.0294
15 5 1 -2.3049 -0.0543
15 5 2 -1.6157 0.2306
15 5 3 2.2185 0.2868
15 5 4 -1.9558 -0.0826
15 5 5 -1.8156 -0.0489
15 5 6 -4.0075 0.0963
15 5 7 -1.5451 -0.0173
15 5 8 1.7681 -0.2482
15 5 9 -0.6971 -0.0088
15 5 10 -1.7858 -0.0040
15 5 11 -7.7488 0.1640
15 5 12 -5.9904 0.0164
15 6 0 1.4966 0.1728
15 6 1 -0.9015 0.0993
15 6 2 -1.9637 0.0167
15 6 3 -2.4167 0.1124
15 6 4 -2.9571 0.1830
15 6 5 -7.2484 -0.0958
15 6 6 -3.8133 -0.1501
15 6 7 -7.8143 -0.0022
15 6 8 -5.9818 -0.0035
15 6 9 8.4937 -0.0786
15 6 10 6.9886 0.2221
15 6 11 -5.9913 -0.0463
15 6 12 -12.4557 -0.1878
15 7 0 -2.5028 -0.0845
15 7 1 1.2641 0.2792
15 7 2 -1.8693 0.0661
15 7 3 -1.5185 -0.0171
15 7 4 -8.3847 0.0257
15 7 5 -7.7260 -0.0226
15 7 6 0.1458 -0.1467
15 7 7 1.8016 -0.0523
15 7 8 -11.8295 0.1766
15 7 9 -7.9198 0.1228
15 7 10 14.4011 -0.0994
15 7 11 8.9743 0.0020
15 7 12 -9.9417 -0.2111
15 8 0 -2.0221 -0.0006
15 8 1 0.5446 -0.1636
15 8 2 -1.5964 0.1164
15 8 3 -4.9528 -0.0274
15 8 4 -2.7717 -0.0499
15 8 5 -3.0117 0.0937
15 8 6 4.8894 -0.0318
15 8 7 6.9342 -0.0047
15 8 8 -8.4154 0.0965
15 8 9 -19.4725 0.0197
15 8 10 1.8725 -0.0965
15 9 1 3.9465 -0.1155
15 9 2 -4.1594 -0.3972
15 9 3 -5.3318 -0.0535
15 9 5 5.6248 0.0818
15 9 6 2.1176 0.2790
15 9 7 3.8528 0.0024
15 9 8 -2.6376 -0.0765
15 9 9 -10.9786 -0.0072
15 10 6 1.0259 0.2326
15 10 7 -2.4766 0.3621
16 -2 0 4.6959 -0.2616
16 -1 0 -0.3629 -0.2325
16 -1 1 5.4449 -0.1691
16 0 0 1.7347 -0.3456
16 0 1 -2.4931 -0.0598
16 0 2 5.6852 -0.2322
16 0 3 1.3524 0.2089
16 1 0 4.3780 0.1912
16 1 1 1.3369 -0.3175
16 1 2 -4.9158 0.1233
16 1 3 6.3600 -0.0527
16 2 0 4.7905 0.3949
16 2 1 2.6674 0.2051
16 2 2 -0.4683 -0.1963
16 2 3 -5.4389 0.1084
16 2 4 1.7695 -0.0168
16 3 0 5.6643 0.0735
16 3 1 6.9074 0.3267
16 3 2 -1.9935 0.0138
16 3 3 -4.4919 -0.2197
16 3 4 -6.3057 0.0393
16 3 5 -0.3160 0.1308
16 3 6 8.1770 -0.1527
16 3 7 13.8280 -0.0065
16 3 8 4.8554 0.0460
16 3 9 -12.7439 0.0383
16 4 0 -5.6730 -0.0862
16 4 1 5.6255 0.0662
16 4 2 5.9773 0.1742
16 4 3 -4.2487 -0.1612
16 4 4 -0.5859 -0.0621
16 4 5 -0.3333 0.0635
16 4 6 1.8730 0.1146
16 4 7 15.1534 -0.1609
16 4 8 22.1296 0.1117
16 4 9 3.7497 0.2266
16 4 10 -17.3050 -0.1813
16 5 1 -1.0901 -0.0461
16 5 2 7.9827 0.1441
16 5 3 5.1517 0.1399
16 5 4 0.5999 -0.2422
16 5 5 7.2190 0.0486
16 5 6 2.8709 0.0780
16 6 1 -5.9470 -0.5802
16 6 2 4.1212 0.2248
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
1.res created by SHELXL-2014/7
TITL 1_a.res in P-1
REM Old TITL 1 in P-1
REM SHELXT solution in P-1
REM R1 0.170, Rweak 0.017, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C38 N12 O44 Co Cu4 Mo10
CELL 0.71073 12.1598 14.1021 23.8608 78.079 82.282 83.825
ZERR 2 0.0005 0.0006 0.0012 0.004 0.004 0.003
LATT 1
SFAC C H Co Cu Mo N O
UNIT 64 96 4 6 20 16 100
SIMU 0.01 0.02 3.8 $O
ISOR 0.001 0.002 O44
L.S. 30 0 0
PLAN 5
list 4
omit-2 53
ABIN
fmap 2 53
acta
OMIT -1 0 3
OMIT 0 -2 1
OMIT 1 -1 2
OMIT 2 0 0
OMIT 7 6 5
OMIT 1 -2 1
OMIT 2 0 2
OMIT 6 6 4
OMIT 0 9 5
REM
REM
REM
WGHT 0.087100 116.298096
FVAR 0.13047
C1 1 0.377727 0.443356 0.911042 11.00000 0.02235 0.02157 =
0.04548 0.00210 -0.00229 -0.00396
AFIX 43
H1 2 0.386765 0.507492 0.892850 11.00000 -1.20000
AFIX 0
C2 1 0.452877 0.283666 0.942882 11.00000 0.03470 0.04099 =
0.03188 -0.00530 0.00380 0.00930
AFIX 43
H2 2 0.514097 0.238032 0.945409 11.00000 -1.20000
AFIX 0
C3 1 0.352072 0.255938 0.966124 11.00000 0.01662 0.02002 =
0.04748 -0.00181 0.00624 -0.00280
AFIX 43
H3 2 0.344778 0.192363 0.985863 11.00000 -1.20000
AFIX 0
C4 1 0.259457 0.320546 0.961058 11.00000 0.02698 0.03726 =
0.05242 -0.01418 0.00022 -0.00736
AFIX 43
H4 2 0.188959 0.301061 0.975921 11.00000 -1.20000
AFIX 0
C5 1 0.273871 0.415979 0.933088 11.00000 0.01733 0.03802 =
0.03757 -0.00636 -0.00390 -0.00893
C6 1 0.175472 0.492389 0.920727 11.00000 0.02901 0.03846 =
0.04408 0.00322 0.00408 0.00911
C7 1 -0.002217 0.573330 0.947658 11.00000 0.02790 0.05195 =
0.03736 0.00047 0.00224 0.01358
AFIX 23
H7A 2 -0.003657 0.589664 0.906215 11.00000 -1.20000
H7B 2 -0.001090 0.633147 0.961552 11.00000 -1.20000
AFIX 0
C8 1 0.103577 0.476596 1.024491 11.00000 0.02035 0.03812 =
0.03523 -0.00372 -0.01619 0.00288
AFIX 23
H8A 2 0.108490 0.532738 1.041368 11.00000 -1.20000
H8B 2 0.169476 0.432595 1.031448 11.00000 -1.20000
AFIX 0
C9 1 0.658655 0.362223 0.999710 11.00000 0.03049 0.02456 =
0.03663 -0.00079 -0.00166 -0.00291
AFIX 43
H9 2 0.594935 0.403646 1.005083 11.00000 -1.20000
AFIX 0
C10 1 0.792558 0.291924 0.937914 11.00000 0.02157 0.03922 =
0.03078 0.00104 -0.00374 -0.00458
AFIX 43
H10 2 0.821183 0.284170 0.900836 11.00000 -1.20000
AFIX 0
C11 1 0.713622 0.318650 1.047297 11.00000 0.02813 0.03936 =
0.03825 -0.00724 -0.00637 -0.00203
AFIX 43
H11 2 0.684424 0.327931 1.084023 11.00000 -1.20000
AFIX 0
C12 1 0.812060 0.261442 1.039388 11.00000 0.05137 0.03258 =
0.04010 0.00579 -0.01186 -0.00838
AFIX 43
H12 2 0.851073 0.233193 1.070451 11.00000 -1.20000
AFIX 0
C13 1 0.851172 0.247141 0.984556 11.00000 0.03390 0.02071 =
0.04438 -0.00019 -0.00917 -0.01427
C14 1 0.964604 0.194603 0.968467 11.00000 0.03524 0.03804 =
0.04796 -0.00371 -0.01224 -0.00091
C15 1 1.095180 0.052818 0.983695 11.00000 0.04084 0.03524 =
0.06975 -0.00592 0.00214 0.00416
AFIX 23
H15A 2 1.128765 0.043685 1.019278 11.00000 -1.20000
H15B 2 1.140620 0.094143 0.953983 11.00000 -1.20000
AFIX 0
C16 1 1.094661 -0.040962 0.967553 11.00000 0.05033 0.03277 =
0.07352 -0.00819 0.00713 0.00457
AFIX 23
H16A 2 1.168665 -0.074363 0.967897 11.00000 -1.20000
H16B 2 1.073839 -0.031619 0.928822 11.00000 -1.20000
AFIX 0
CO1 3 0.768100 0.656621 0.670210 11.00000 0.01908 0.01677 =
0.02928 -0.00001 -0.00209 0.00041
CO2 3 0.788803 0.735347 0.766020 11.00000 0.01933 0.02046 =
0.02991 -0.00170 -0.00260 -0.00317
CU1 4 0.620477 0.411779 0.876618 11.00000 0.01911 0.03001 =
0.03417 0.00574 -0.00192 -0.00023
CU2 4 0.168531 0.480639 0.795790 11.00000 0.07457 0.09774 =
0.07668 0.00447 -0.00467 -0.01111
MO1 5 0.583663 0.611794 0.765050 11.00000 0.01571 0.02273 =
0.02956 0.00036 -0.00323 -0.00069
MO2 5 0.615987 0.686366 0.882262 11.00000 0.02685 0.02646 =
0.02962 -0.00358 -0.00133 -0.00064
MO3 5 0.816395 0.827851 0.880033 11.00000 0.03666 0.02673 =
0.03591 -0.00544 -0.00895 -0.00200
MO4 5 0.995478 0.869210 0.763785 11.00000 0.02803 0.03048 =
0.04536 0.00185 -0.00790 -0.00835
MO5 5 0.973448 0.770802 0.652649 11.00000 0.01987 0.03601 =
0.03502 0.00310 -0.00271 -0.00489
MO6 5 0.723920 0.892057 0.665262 11.00000 0.02698 0.01986 =
0.03854 -0.00019 -0.00716 -0.00135
MO7 5 0.719550 0.804347 0.548891 11.00000 0.02655 0.02519 =
0.03139 0.00185 -0.00572 -0.00074
MO8 5 0.750956 0.565279 0.554690 11.00000 0.03072 0.02771 =
0.03248 -0.00475 -0.00423 -0.00105
MO9 5 0.800638 0.423562 0.677639 11.00000 0.02870 0.01994 =
0.03370 -0.00425 -0.00163 -0.00108
MO10 5 0.844364 0.521340 0.785834 11.00000 0.01830 0.02091 =
0.02960 -0.00022 -0.00318 0.00073
N1 6 0.468114 0.377609 0.915459 11.00000 0.01412 0.04261 =
0.03942 0.00281 -0.00685 -0.00210
N2 6 0.099291 0.508212 0.961457 11.00000 0.02110 0.05050 =
0.03145 -0.00152 -0.00658 0.00989
N3 6 0.694497 0.346523 0.946055 11.00000 0.01796 0.02990 =
0.03704 -0.00298 -0.00401 -0.00160
N4 6 0.985463 0.100556 0.991450 11.00000 0.01534 0.03460 =
0.06730 0.00493 0.00471 -0.00355
O1 7 0.490642 0.630882 0.716259 11.00000 0.03228 0.03360 =
0.03850 0.00272 -0.00880 0.00034
O50 7 0.630115 0.273282 0.837003 11.00000 0.05046 0.06473 =
0.05588 -0.01283 0.01285 -0.00705
AFIX 7
H50A 2 0.612806 0.223071 0.863821 11.00000 -1.50000
H50B 2 0.698750 0.256997 0.823884 11.00000 -1.50000
AFIX 0
O2 7 0.555234 0.499205 0.810594 11.00000 0.02421 0.02890 =
0.03980 -0.00208 -0.00681 -0.00157
O3 7 0.530618 0.693002 0.816612 11.00000 0.02652 0.02457 =
0.03708 -0.00684 -0.00451 0.00073
O4 7 0.731553 0.622613 0.812252 11.00000 0.02164 0.02728 =
0.03437 -0.00079 -0.00272 -0.00160
O5 7 0.592372 0.570124 0.917782 11.00000 0.03974 0.02857 =
0.04009 0.00341 -0.00216 -0.00919
O6 7 0.524426 0.759352 0.915924 11.00000 0.03947 0.04409 =
0.04007 -0.00914 0.00208 -0.00469
O7 7 0.750241 0.705478 0.909364 11.00000 0.02549 0.03387 =
0.03705 -0.00170 -0.00882 -0.00093
O8 7 0.694344 0.808428 0.817275 11.00000 0.02408 0.02336 =
0.03766 -0.00722 -0.00546 -0.00048
O9 7 0.723249 0.907184 0.911685 11.00000 0.04050 0.03240 =
0.05303 -0.01305 -0.00733 0.00028
O10 7 0.923870 0.802716 0.921270 11.00000 0.04371 0.04087 =
0.04884 -0.00877 -0.01780 -0.00082
O11 7 0.876458 0.919953 0.814005 11.00000 0.03282 0.02962 =
0.04746 -0.00178 -0.00921 -0.00286
O12 7 0.904917 0.740538 0.813299 11.00000 0.02519 0.03077 =
0.03729 -0.00054 -0.00745 -0.00241
O13 7 1.098848 0.849042 0.806213 11.00000 0.03763 0.04502 =
0.06033 -0.00412 -0.01543 -0.00433
O14 7 1.018193 0.976929 0.715958 11.00000 0.04248 0.04541 =
0.06186 0.00255 -0.00473 -0.01663
O15 7 0.847246 0.844437 0.713582 11.00000 0.02332 0.02733 =
0.03932 -0.00209 -0.00634 -0.00366
O16 7 1.050873 0.772764 0.716335 11.00000 0.02723 0.03023 =
0.04552 0.00078 -0.00253 -0.00766
O17 7 1.014376 0.871972 0.606633 11.00000 0.02785 0.04259 =
0.05290 0.01182 -0.00883 -0.00710
O18 7 1.044500 0.674088 0.624918 11.00000 0.02316 0.04881 =
0.04803 -0.00550 0.00359 0.00272
O19 7 0.874210 0.650463 0.721719 11.00000 0.02241 0.02587 =
0.03499 -0.00112 -0.00208 -0.00102
O20 7 0.679157 0.732697 0.717447 11.00000 0.02264 0.02265 =
0.03482 -0.00261 -0.00378 -0.00441
O21 7 0.626072 0.936038 0.714570 11.00000 0.04545 0.03003 =
0.04666 -0.01322 -0.01464 0.01313
O22 7 0.787685 0.991351 0.627042 11.00000 0.04142 0.02240 =
0.05378 0.00089 -0.00841 -0.00789
O23 7 0.826660 0.773683 0.625092 11.00000 0.02304 0.02544 =
0.03608 -0.00059 -0.00064 -0.00253
O24 7 0.641249 0.867746 0.609975 11.00000 0.03093 0.02633 =
0.03755 0.00018 -0.00360 0.00058
O25 7 0.804689 0.891354 0.512738 11.00000 0.03567 0.03585 =
0.04458 0.00970 0.00116 -0.00362
O26 7 0.610710 0.814320 0.508768 11.00000 0.03013 0.03717 =
0.04398 0.00044 -0.01083 -0.00310
O27 7 0.807126 0.691597 0.525751 11.00000 0.03011 0.03209 =
0.03484 0.00152 -0.00062 -0.00245
O28 7 0.854971 0.566437 0.627561 11.00000 0.02378 0.02476 =
0.03208 -0.00050 -0.00084 0.00057
O29 7 0.666425 0.667915 0.612627 11.00000 0.02198 0.02304 =
0.03375 0.00055 -0.00302 -0.00404
O30 7 0.856023 0.498255 0.521296 11.00000 0.04513 0.04318 =
0.03984 -0.00482 -0.00528 -0.00222
O31 7 0.641053 0.570786 0.515840 11.00000 0.04482 0.03914 =
0.03869 -0.00397 -0.00967 -0.00472
O32 7 0.699839 0.470199 0.622016 11.00000 0.02900 0.02688 =
0.03739 -0.00108 -0.00111 -0.00099
O33 7 0.897736 0.354276 0.641998 11.00000 0.03758 0.03009 =
0.04212 -0.00060 0.00105 -0.00468
O34 7 0.724127 0.340749 0.724748 11.00000 0.03430 0.03398 =
0.04016 -0.00645 -0.00180 -0.00538
O35 7 0.903479 0.450505 0.730087 11.00000 0.02536 0.02404 =
0.03591 -0.00149 -0.00270 0.00068
O36 7 0.716002 0.546013 0.721908 11.00000 0.02205 0.02158 =
0.03362 -0.00388 -0.00234 -0.00473
O37 7 0.960431 0.533620 0.818277 11.00000 0.02376 0.03763 =
0.04158 -0.00273 -0.00496 -0.00303
O38 7 0.770534 0.434944 0.834568 11.00000 0.02556 0.02258 =
0.03429 0.00064 -0.00124 0.00136
O39 7 1.034036 0.242759 0.935618 11.00000 0.03131 0.04712 =
0.06592 0.01818 0.00448 0.00315
O40 7 0.169526 0.530345 0.869621 11.00000 0.04376 0.08996 =
0.04336 0.00490 0.00142 0.00565
O43 7 0.197085 0.612279 0.755398 11.00000 0.05857 0.08022 =
0.08035 0.00856 -0.00515 -0.00974
AFIX 7
H43A 2 0.270219 0.624975 0.751702 11.00000 -1.50000
H43B 2 0.164711 0.658728 0.775354 11.00000 -1.50000
AFIX 0
O44 7 0.347072 0.429765 0.778001 11.00000 0.09164 0.09311 =
0.09227 -0.01645 -0.00949 -0.00710
AFIX 7
H44A 2 0.373160 0.423819 0.737908 11.00000 -1.50000
H44B 2 0.367491 0.362547 0.796737 11.00000 -1.50000
AFIX 0
O45 7 0.133496 0.444926 0.724908 11.00000 0.08431 0.09319 =
0.08961 -0.01564 -0.00058 -0.01311
AFIX 7
H45A 2 0.160969 0.379668 0.718890 11.00000 -1.50000
H45B 2 0.167692 0.481187 0.688162 11.00000 -1.50000
AFIX 0
O46 7 0.126487 0.350709 0.834807 11.00000 0.10584 0.09215 =
0.09553 0.00075 0.01139 -0.00791
AFIX 7
H46A 2 0.150117 0.304218 0.813654 11.00000 -1.50000
H46B 2 0.051533 0.345429 0.840002 11.00000 -1.50000
AFIX 0
C17 1 0.700421 0.242117 0.608794 11.00000 0.03705 0.06397 =
0.05617 -0.02316 -0.00344 -0.01276
AFIX 43
H 2 0.713683 0.234631 0.647014 11.00000 -1.20000
AFIX 0
C18 1 0.763025 0.235783 0.515235 11.00000 0.04491 0.04951 =
0.03858 -0.00457 -0.01029 -0.00663
AFIX 43
HA 2 0.821201 0.227412 0.486663 11.00000 -1.20000
AFIX 0
C19 1 0.593616 0.263360 0.595738 11.00000 0.03902 0.07315 =
0.07696 -0.03089 -0.00546 -0.01650
AFIX 43
HB 2 0.535799 0.273797 0.624097 11.00000 -1.20000
AFIX 0
C20 1 0.573455 0.268949 0.540667 11.00000 0.02886 0.09072 =
0.10350 -0.05288 -0.02031 0.00575
AFIX 43
HC 2 0.501640 0.284639 0.530409 11.00000 -1.20000
AFIX 0
C21 1 0.657629 0.251722 0.501485 11.00000 0.02615 0.03890 =
0.07753 -0.01083 -0.01978 -0.02000
C22 1 0.640863 0.262866 0.438244 11.00000 0.04701 0.05308 =
0.06830 0.01135 -0.01711 -0.00513
C23 1 0.682196 0.208190 0.346185 11.00000 0.02190 0.02954 =
0.06419 0.00593 -0.00007 0.00134
AFIX 23
HD 2 0.655100 0.274878 0.331828 11.00000 -1.20000
HE 2 0.758380 0.198600 0.328843 11.00000 -1.20000
AFIX 0
C24 1 0.616105 0.144572 0.328862 11.00000 0.04526 0.05245 =
0.04369 0.00456 0.00251 0.00340
AFIX 23
HF 2 0.625686 0.152551 0.287179 11.00000 -1.20000
HG 2 0.538050 0.159555 0.341321 11.00000 -1.20000
AFIX 0
C25 1 0.716069 0.091291 0.435695 11.00000 0.04910 0.03947 =
0.04900 0.00406 -0.00831 -0.00488
AFIX 23
HH 2 0.706193 0.083530 0.477368 11.00000 -1.20000
HI 2 0.794112 0.075933 0.423390 11.00000 -1.20000
AFIX 0
C26 1 0.645432 0.024124 0.417183 11.00000 0.02736 0.04296 =
0.05476 -0.00259 0.00846 -0.01161
AFIX 23
HJ 2 0.671770 -0.042970 0.431013 11.00000 -1.20000
HK 2 0.568744 0.034134 0.433709 11.00000 -1.20000
AFIX 0
C27 1 0.691755 -0.020092 0.323044 11.00000 0.06128 0.03451 =
0.05729 -0.00953 -0.01584 0.00938
C28 1 0.741061 -0.117221 0.349548 11.00000 0.04603 0.06386 =
0.02922 -0.00227 -0.00857 0.00146
C29 1 0.844943 -0.125402 0.371147 11.00000 0.02730 0.03761 =
0.05485 0.00339 -0.01570 0.00663
AFIX 43
HL 2 0.876855 -0.068872 0.372263 11.00000 -1.20000
AFIX 0
C30 1 0.849164 -0.292272 0.389499 11.00000 0.04323 0.03961 =
0.06304 -0.00853 -0.00199 0.00261
AFIX 43
HM 2 0.884792 -0.352361 0.403936 11.00000 -1.20000
AFIX 0
C31 1 0.748358 -0.291984 0.368922 11.00000 0.03236 0.04624 =
0.10638 -0.02141 -0.01533 -0.00887
AFIX 43
HN 2 0.716113 -0.349255 0.369851 11.00000 -1.20000
AFIX 0
C32 1 0.698136 -0.202252 0.346941 11.00000 0.04637 0.07570 =
0.07834 -0.02552 -0.01761 0.00028
AFIX 43
HO 2 0.633170 -0.199079 0.329803 11.00000 -1.20000
AFIX 0
CU3 4 0.944177 0.219437 0.588538 11.00000 0.02756 0.02577 =
0.04311 -0.00163 -0.00274 -0.00390
N5 6 0.785827 0.231731 0.569405 11.00000 0.01810 0.03035 =
0.06310 -0.01232 -0.00852 -0.00483
N6 6 0.680901 0.193034 0.408795 11.00000 0.03800 0.02501 =
0.06432 0.00019 -0.01406 -0.00138
N7 6 0.651539 0.043349 0.355320 11.00000 0.04182 0.03889 =
0.04538 -0.00141 -0.00959 -0.00731
N8 6 0.900008 -0.212507 0.390333 11.00000 0.03468 0.02236 =
0.03673 -0.00490 0.00823 -0.00065
O41 7 0.584988 0.337751 0.413799 11.00000 0.09906 0.05851 =
0.08609 -0.00417 -0.02831 0.03033
O42 7 0.685736 -0.003684 0.269549 11.00000 0.10971 0.09953 =
0.04702 -0.01819 -0.02435 0.05088
O47 7 0.893017 0.136639 0.662985 11.00000 0.04944 0.05127 =
0.06232 0.00947 0.00845 0.00092
AFIX 7
HP 2 0.923620 0.148434 0.693200 11.00000 -1.50000
HQ 2 0.916360 0.073341 0.664104 11.00000 -1.50000
AFIX 0
O48 7 0.982089 0.317864 0.517363 11.00000 0.03347 0.02719 =
0.04453 0.00722 -0.00273 0.00072
AFIX 7
HR 2 0.941112 0.372128 0.518283 11.00000 -1.50000
HS 2 0.964218 0.299921 0.487234 11.00000 -1.50000
AFIX 0
O49 7 0.979776 0.086805 0.543603 11.00000 0.04599 0.02961 =
0.06385 -0.00104 -0.00423 -0.01271
AFIX 7
HT 2 0.919368 0.074697 0.531688 11.00000 -1.50000
HU 2 0.996316 0.034380 0.568316 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1_a.res in P-1
REM R1 = 0.0923 for 11050 Fo > 4sig(Fo) and 0.1279 for all 16348 data
REM 954 parameters refined using 1020 restraints
END
WGHT 0.0847 124.3127
REM Highest difference peak 1.606, deepest hole -2.842, 1-sigma level 0.275
Q1 1 0.7613 0.5602 0.5205 11.00000 0.05 1.61
Q2 1 0.5836 0.6248 0.7226 11.00000 0.05 1.51
Q3 1 0.7192 0.7959 0.5860 11.00000 0.05 1.47
Q4 1 0.9947 0.8760 0.7200 11.00000 0.05 1.43
Q5 1 0.9893 0.7786 0.6070 11.00000 0.05 1.40
REM The information below was added by Olex2.
REM
REM R1 = 0.0923 for 11050 Fo > 4sig(Fo) and 0.1279 for all 40618 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.61, deepest hole -2.84
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.1279
REM R1_gt = 0.0923
REM wR_ref = 0.2481
REM GOOF = 1.060
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 40618
REM Reflections_gt = 11050
REM Parameters = n/a
REM Hole = -2.84
REM Peak = 1.61
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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1885054'
loop_
_audit_author_name
_audit_author_address
'Fengcai Li'
;Zhengzhou University of Light Industry
China
;
_audit_update_record
;
2018-12-14 deposited with the CCDC. 2019-04-01 downloaded from the CCDC.
;
_audit_creation_date 2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'0.5(C32 H56 Co4 Mo20 N8 O96 Zn4), C16 H16 N4 O2'
_chemical_formula_sum 'C32 H44 Co2 Mo10 N8 O50 Zn2'
_chemical_formula_weight 2548.75
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 21.544(2)
_cell_length_b 14.2328(12)
_cell_length_c 24.246(3)
_cell_angle_alpha 90
_cell_angle_beta 104.817(10)
_cell_angle_gamma 90
_cell_volume 7187.6(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 8085
_cell_measurement_temperature 298.15
_cell_measurement_theta_max 29.3350
_cell_measurement_theta_min 4.0170
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.889
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.46922
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear dark green'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 2.355
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 4904
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0637
_diffrn_reflns_av_unetI/netI 0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 17793
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.994
_diffrn_reflns_theta_min 3.648
_diffrn_ambient_temperature 298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Xcalibur, Eos, Gemini'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5513
_reflns_number_total 7033
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 3.009
_refine_diff_density_min -2.305
_refine_diff_density_rms 0.272
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.091
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 472
_refine_ls_number_reflns 7033
_refine_ls_number_restraints 24
_refine_ls_R_factor_all 0.1109
_refine_ls_R_factor_gt 0.0921
_refine_ls_restrained_S_all 1.090
_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^)+(0.0456P)^2^+642.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2025
_refine_ls_wR_factor_ref 0.2129
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
O22(H22A,H22B), O23(H23A,H23B), O24(H24A,H24B)
3.b Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B)
3.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6728(8) 0.1609(14) 0.4964(8) 0.050(5) Uani 1 1 d . . . . .
H1 H 0.7099 0.1289 0.4945 0.060 Uiso 1 1 calc R . . . .
C2 C 0.6700(9) 0.2008(18) 0.5470(8) 0.067(6) Uani 1 1 d . . . . .
H2 H 0.7032 0.1912 0.5795 0.080 Uiso 1 1 calc R . . . .
C3 C 0.6181(8) 0.2550(14) 0.5497(8) 0.050(5) Uani 1 1 d . . . . .
H3 H 0.6170 0.2865 0.5831 0.060 Uiso 1 1 calc R . . . .
C4 C 0.5678(7) 0.2614(11) 0.5016(7) 0.036(4) Uani 1 1 d . . . . .
C5 C 0.5733(8) 0.2164(13) 0.4529(7) 0.042(4) Uani 1 1 d . . . . .
H5 H 0.5396 0.2209 0.4202 0.051 Uiso 1 1 calc R . . . .
C6 C 0.5053(8) 0.3115(12) 0.5008(7) 0.039(4) Uani 1 1 d . . . . .
C7 C 0.5640(7) 0.4646(12) 0.5219(7) 0.037(4) Uani 1 1 d . . . . .
H7A H 0.6002 0.4294 0.5158 0.044 Uiso 1 1 calc R . . . .
H7B H 0.5750 0.4865 0.5611 0.044 Uiso 1 1 calc R . . . .
C8 C 0.4489(8) 0.4518(12) 0.5180(7) 0.039(4) Uani 1 1 d . . . . .
H8A H 0.4542 0.4726 0.5570 0.046 Uiso 1 1 calc R . . . .
H8B H 0.4130 0.4085 0.5084 0.046 Uiso 1 1 calc R . . . .
Co1 Co 0.43332(8) 0.53755(12) 0.23211(7) 0.0163(4) Uani 1 1 d . . . . .
Mo1 Mo 0.49114(6) 0.69455(9) 0.17973(5) 0.0266(3) Uani 1 1 d . . . . .
Mo2 Mo 0.64754(6) 0.69993(10) 0.22443(6) 0.0314(3) Uani 1 1 d . . . . .
Mo3 Mo 0.72452(5) 0.53691(9) 0.31182(5) 0.0265(3) Uani 1 1 d . . . . .
Mo4 Mo 0.63923(5) 0.37437(9) 0.35745(5) 0.0227(3) Uani 1 1 d . . . . .
Mo5 Mo 0.48266(5) 0.38455(8) 0.31336(5) 0.0195(3) Uani 1 1 d . . . . .
N1 N 0.6255(6) 0.1661(10) 0.4506(5) 0.036(3) Uani 1 1 d . . . . .
N2 N 0.5083(6) 0.4041(10) 0.5123(6) 0.037(3) Uani 1 1 d . . . . .
O1 O 0.4348(5) 0.6669(8) 0.1182(5) 0.039(3) Uani 1 1 d . . . . .
O2 O 0.4864(6) 0.8141(9) 0.1841(5) 0.047(3) Uani 1 1 d . . . . .
O3 O 0.5715(4) 0.6831(7) 0.1624(4) 0.031(2) Uani 1 1 d . . . . .
O4 O 0.6435(5) 0.8192(9) 0.2362(5) 0.051(3) Uani 1 1 d . . . . .
O5 O 0.7021(5) 0.6915(8) 0.1846(4) 0.042(3) Uani 1 1 d . . . . .
O6 O 0.7004(5) 0.6660(7) 0.2993(4) 0.029(2) Uani 1 1 d . . . . .
O7 O 0.7748(5) 0.5238(8) 0.2683(5) 0.040(3) Uani 1 1 d . . . . .
O8 O 0.7727(5) 0.5472(9) 0.3779(5) 0.048(3) Uani 1 1 d . . . . .
O9 O 0.6991(4) 0.4074(7) 0.3138(4) 0.026(2) Uani 1 1 d . . . . .
O10 O 0.6855(4) 0.3850(8) 0.4252(4) 0.036(2) Uani 1 1 d . . . . .
O11 O 0.6338(5) 0.2568(7) 0.3428(4) 0.032(2) Uani 1 1 d . U . . .
O12 O 0.5585(4) 0.3973(7) 0.3732(4) 0.023(2) Uani 1 1 d . . . . .
O13 O 0.4809(4) 0.2657(7) 0.3068(4) 0.026(2) Uani 1 1 d . U . . .
O14 O 0.4239(5) 0.4130(7) 0.3461(4) 0.029(2) Uani 1 1 d . . . . .
O15 O 0.4967(4) 0.5363(7) 0.3000(3) 0.0214(19) Uani 1 1 d . . . . .
O16 O 0.4378(4) 0.4065(7) 0.2323(4) 0.026(2) Uani 1 1 d . . . . .
O17 O 0.3634(4) 0.5446(7) 0.2668(4) 0.028(2) Uani 1 1 d . . . . .
O18 O 0.3671(4) 0.5268(6) 0.1593(4) 0.0208(19) Uani 1 1 d . . . . .
O19 O 0.4371(4) 0.6703(6) 0.2341(4) 0.0197(18) Uani 1 1 d . U . . .
O20 O 0.4553(5) 0.2670(9) 0.4901(6) 0.050(3) Uani 1 1 d . . . . .
O22 O 0.5373(7) 0.1019(10) 0.3359(7) 0.076(5) Uani 1 1 d . . . . .
H22A H 0.5287 0.0854 0.2988 0.114 Uiso 1 1 d GR . . . .
H22B H 0.5170 0.1579 0.3337 0.114 Uiso 1 1 d GR . . . .
O23 O 0.6368(9) 0.0560(14) 0.2917(9) 0.098(6) Uani 1 1 d . . . . .
H23A H 0.6002 0.0218 0.2733 0.147 Uiso 1 1 d GR . . . .
H23B H 0.6684 0.0098 0.2932 0.147 Uiso 1 1 d GR . . . .
O24 O 0.7287(6) 0.1058(10) 0.3875(7) 0.067(4) Uani 1 1 d . . . . .
H24A H 0.7420 0.1058 0.3552 0.101 Uiso 1 1 d GR . . . .
H24B H 0.7453 0.0515 0.4036 0.101 Uiso 1 1 d GR . . . .
O25 O 0.6283(9) -0.0307(13) 0.3996(8) 0.089(5) Uani 1 1 d . U . . .
Zn1 Zn 0.63262(9) 0.11053(15) 0.37294(9) 0.0437(5) Uani 1 1 d . . . . .
C9 C 0.6607(7) 0.2378(13) 0.2120(7) 0.043(4) Uani 1 1 d . . . . .
H9 H 0.6483 0.2118 0.2428 0.051 Uiso 1 1 calc R . . . .
C10 C 0.6399(7) 0.1970(12) 0.1581(6) 0.036(3) Uani 1 1 d . . . . .
H10 H 0.6142 0.1435 0.1518 0.043 Uiso 1 1 calc R . . . .
C11 C 0.6592(7) 0.2401(12) 0.1153(6) 0.036(4) Uani 1 1 d . . . . .
H11 H 0.6445 0.2164 0.0785 0.043 Uiso 1 1 calc R . . . .
C12 C 0.6997(6) 0.3176(11) 0.1235(6) 0.026(3) Uani 1 1 d . . . . .
C13 C 0.7187(7) 0.3503(12) 0.1769(7) 0.036(4) Uani 1 1 d . . . . .
H13 H 0.7472 0.4006 0.1846 0.044 Uiso 1 1 calc R . . . .
C14 C 0.7200(7) 0.3650(11) 0.0767(7) 0.032(3) Uani 1 1 d . . . . .
C15 C 0.7749(9) 0.2206(12) 0.0570(7) 0.045(4) Uani 1 1 d . . . . .
H15A H 0.7687 0.1996 0.0932 0.054 Uiso 1 1 calc R . . . .
H15B H 0.8207 0.2261 0.0608 0.054 Uiso 1 1 calc R . . . .
C16 C 0.7537(9) 0.3511(11) -0.0110(7) 0.043(4) Uani 1 1 d . . . . .
H16A H 0.7990 0.3604 -0.0083 0.052 Uiso 1 1 calc R . . . .
H16B H 0.7318 0.4109 -0.0193 0.052 Uiso 1 1 calc R . . . .
N3 N 0.6980(6) 0.3134(10) 0.2198(5) 0.037(3) Uani 1 1 d . . . . .
N4 N 0.7446(7) 0.3116(10) 0.0427(5) 0.039(3) Uani 1 1 d . . . . .
O21 O 0.7076(5) 0.4479(8) 0.0689(5) 0.041(3) 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
C1 0.033(8) 0.065(13) 0.055(11) 0.010(10) 0.013(8) 0.017(8)
C2 0.049(11) 0.101(18) 0.042(10) -0.002(11) -0.004(8) 0.038(12)
C3 0.033(8) 0.067(13) 0.043(10) -0.019(9) -0.005(7) 0.008(8)
C4 0.033(8) 0.036(9) 0.038(9) 0.021(7) 0.007(6) 0.000(7)
C5 0.034(8) 0.054(11) 0.040(9) 0.023(8) 0.012(7) 0.007(8)
C6 0.041(9) 0.041(10) 0.035(8) 0.016(7) 0.008(7) -0.005(7)
C7 0.024(7) 0.043(9) 0.040(9) -0.001(7) 0.003(6) 0.002(7)
C8 0.040(8) 0.035(9) 0.044(9) 0.004(7) 0.018(7) 0.009(7)
Co1 0.0164(7) 0.0140(8) 0.0200(8) 0.0010(7) 0.0075(6) 0.0023(6)
Mo1 0.0308(6) 0.0245(6) 0.0275(6) 0.0032(5) 0.0129(5) -0.0026(5)
Mo2 0.0287(6) 0.0314(7) 0.0375(7) 0.0015(6) 0.0148(5) -0.0114(5)
Mo3 0.0194(5) 0.0319(7) 0.0300(6) -0.0069(5) 0.0097(5) -0.0075(5)
Mo4 0.0172(5) 0.0279(6) 0.0236(6) 0.0020(5) 0.0061(4) 0.0040(4)
Mo5 0.0170(5) 0.0192(6) 0.0233(6) 0.0034(5) 0.0073(4) 0.0000(4)
N1 0.037(7) 0.040(8) 0.032(7) 0.011(6) 0.011(5) 0.011(6)
N2 0.022(6) 0.041(8) 0.051(8) -0.002(6) 0.015(6) 0.004(5)
O1 0.039(6) 0.037(6) 0.044(6) 0.006(5) 0.014(5) 0.007(5)
O2 0.063(8) 0.047(7) 0.039(6) 0.007(6) 0.026(6) -0.002(6)
O3 0.023(5) 0.039(6) 0.035(5) 0.001(5) 0.012(4) 0.000(4)
O4 0.037(6) 0.056(8) 0.058(8) 0.002(6) 0.009(6) -0.007(6)
O5 0.042(6) 0.048(7) 0.034(6) -0.002(5) 0.006(5) -0.015(5)
O6 0.035(5) 0.032(6) 0.022(5) -0.005(4) 0.013(4) -0.022(4)
O7 0.026(5) 0.046(7) 0.053(7) -0.017(6) 0.018(5) -0.012(5)
O8 0.034(6) 0.068(9) 0.038(6) -0.027(6) 0.004(5) -0.018(6)
O9 0.028(5) 0.028(5) 0.027(5) -0.012(4) 0.015(4) 0.000(4)
O10 0.020(5) 0.053(7) 0.030(5) 0.002(5) -0.001(4) -0.004(5)
O11 0.033(2) 0.032(2) 0.033(2) 0.0006(10) 0.0082(11) 0.0006(10)
O12 0.021(4) 0.028(5) 0.020(4) 0.012(4) 0.007(3) 0.008(4)
O13 0.026(3) 0.023(3) 0.028(3) 0.0014(18) 0.0071(18) -0.0004(18)
O14 0.032(5) 0.033(6) 0.027(5) 0.010(4) 0.014(4) 0.003(4)
O15 0.023(4) 0.030(5) 0.014(4) -0.010(4) 0.009(3) 0.003(4)
O16 0.023(4) 0.022(5) 0.033(5) 0.006(4) 0.008(4) 0.002(4)
O17 0.019(4) 0.039(6) 0.031(5) -0.004(5) 0.017(4) 0.004(4)
O18 0.019(4) 0.020(5) 0.025(5) 0.010(4) 0.008(4) 0.006(4)
O19 0.020(2) 0.019(2) 0.020(2) -0.0002(10) 0.0055(11) 0.0006(10)
O20 0.028(6) 0.047(7) 0.070(9) -0.007(6) 0.006(5) -0.008(5)
O22 0.060(9) 0.045(9) 0.105(13) -0.005(8) -0.013(8) 0.003(7)
O23 0.082(12) 0.095(14) 0.131(16) -0.012(12) 0.051(12) 0.011(11)
O24 0.048(7) 0.052(8) 0.115(12) 0.039(8) 0.046(8) 0.032(6)
O25 0.089(5) 0.089(5) 0.090(5) 0.002(2) 0.023(2) 0.001(2)
Zn1 0.0380(10) 0.0432(12) 0.0558(12) 0.0141(10) 0.0226(9) 0.0155(9)
C9 0.032(8) 0.057(11) 0.044(9) 0.014(8) 0.020(7) 0.021(8)
C10 0.035(8) 0.037(9) 0.037(8) 0.002(7) 0.013(6) 0.009(7)
C11 0.031(7) 0.045(10) 0.028(8) -0.017(7) 0.002(6) 0.007(7)
C12 0.016(6) 0.036(8) 0.027(7) 0.001(6) 0.004(5) 0.006(6)
C13 0.028(7) 0.040(9) 0.038(8) -0.017(7) 0.005(6) -0.012(7)
C14 0.030(7) 0.026(8) 0.040(8) -0.002(7) 0.011(6) 0.008(6)
C15 0.062(11) 0.042(10) 0.039(9) 0.001(8) 0.029(8) 0.014(8)
C16 0.074(12) 0.026(8) 0.039(9) 0.005(7) 0.031(8) 0.018(8)
N3 0.038(7) 0.048(9) 0.026(6) 0.013(6) 0.009(5) 0.027(6)
N4 0.055(8) 0.033(7) 0.034(7) 0.001(6) 0.021(6) 0.011(6)
O21 0.048(6) 0.035(7) 0.038(6) -0.008(5) 0.010(5) 0.000(5)
_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
C1 C2 1.37(3) . ?
C1 N1 1.30(2) . ?
C2 C3 1.38(2) . ?
C3 C4 1.38(2) . ?
C4 C5 1.37(2) . ?
C4 C6 1.52(2) . ?
C5 N1 1.35(2) . ?
C6 N2 1.35(2) . ?
C6 O20 1.219(19) . ?
C7 C8 1.51(2) 5_666 ?
C7 N2 1.448(19) . ?
C8 C7 1.51(2) 5_666 ?
C8 N2 1.485(18) . ?
Co1 Co1 2.781(3) 2_655 ?
Co1 Mo1 2.995(2) . ?
Co1 Mo5 2.946(2) . ?
Co1 O15 1.864(8) 2_655 ?
Co1 O15 1.850(9) . ?
Co1 O16 1.868(9) . ?
Co1 O17 1.907(8) . ?
Co1 O18 1.972(9) . ?
Co1 O19 1.891(9) . ?
Mo1 O1 1.711(11) . ?
Mo1 O2 1.709(13) . ?
Mo1 O3 1.890(9) . ?
Mo1 O15 2.306(9) 2_655 ?
Mo1 O19 2.285(8) 2_655 ?
Mo1 O19 1.999(8) . ?
Mo2 O3 1.934(10) . ?
Mo2 O4 1.728(14) . ?
Mo2 O5 1.705(11) . ?
Mo2 O6 1.941(10) . ?
Mo2 O17 2.239(10) 2_655 ?
Mo2 O19 2.336(8) 2_655 ?
Mo3 O6 1.913(10) . ?
Mo3 O7 1.706(10) . ?
Mo3 O8 1.678(11) . ?
Mo3 O9 1.927(10) . ?
Mo3 O17 2.322(9) 2_655 ?
Mo3 O18 2.261(8) 2_655 ?
Mo4 O9 1.925(9) . ?
Mo4 O10 1.697(10) . ?
Mo4 O11 1.708(10) . ?
Mo4 O12 1.902(8) . ?
Mo4 O16 2.420(9) 2_655 ?
Mo4 O18 2.206(9) 2_655 ?
Mo5 O12 1.895(9) . ?
Mo5 O13 1.698(10) . ?
Mo5 O14 1.706(9) . ?
Mo5 O15 2.217(10) . ?
Mo5 O16 1.980(9) . ?
Mo5 O16 2.286(9) 2_655 ?
N1 Zn1 2.085(13) . ?
O11 Zn1 2.210(11) . ?
O15 Co1 1.864(8) 2_655 ?
O15 Mo1 2.306(9) 2_655 ?
O16 Mo4 2.420(9) 2_655 ?
O16 Mo5 2.286(9) 2_655 ?
O17 Mo2 2.239(10) 2_655 ?
O17 Mo3 2.322(9) 2_655 ?
O18 Mo3 2.261(8) 2_655 ?
O18 Mo4 2.206(9) 2_655 ?
O19 Mo1 2.285(8) 2_655 ?
O19 Mo2 2.336(8) 2_655 ?
O22 Zn1 2.024(14) . ?
O23 Zn1 2.140(19) . ?
O24 Zn1 2.010(12) . ?
O25 Zn1 2.121(19) . ?
C9 C10 1.40(2) . ?
C9 N3 1.33(2) . ?
C10 C11 1.36(2) . ?
C11 C12 1.39(2) . ?
C12 C13 1.34(2) . ?
C12 C14 1.48(2) . ?
C13 N3 1.34(2) . ?
C14 N4 1.328(19) . ?
C14 O21 1.213(18) . ?
C15 C16 1.52(2) 7_655 ?
C15 N4 1.45(2) . ?
C16 C15 1.52(2) 7_655 ?
C16 N4 1.475(19) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.4(16) . . ?
C1 C2 C3 120.0(17) . . ?
C2 C3 C4 118.0(17) . . ?
C3 C4 C6 123.0(16) . . ?
C5 C4 C3 118.3(15) . . ?
C5 C4 C6 118.6(14) . . ?
N1 C5 C4 122.7(15) . . ?
N2 C6 C4 117.5(14) . . ?
O20 C6 C4 119.4(16) . . ?
O20 C6 N2 123.0(16) . . ?
N2 C7 C8 110.8(13) . 5_666 ?
N2 C8 C7 108.9(13) . 5_666 ?
Co1 Co1 Mo1 67.89(5) 2_655 . ?
Co1 Co1 Mo5 67.92(5) 2_655 . ?
Mo5 Co1 Mo1 135.81(6) . . ?
O15 Co1 Co1 41.7(2) . 2_655 ?
O15 Co1 Co1 41.3(3) 2_655 2_655 ?
O15 Co1 Mo1 95.3(3) . . ?
O15 Co1 Mo1 50.3(3) 2_655 . ?
O15 Co1 Mo5 48.7(3) . . ?
O15 Co1 Mo5 94.6(3) 2_655 . ?
O15 Co1 O15 83.0(4) . 2_655 ?
O15 Co1 O16 87.8(4) . . ?
O15 Co1 O16 86.8(4) 2_655 . ?
O15 Co1 O17 177.1(4) 2_655 . ?
O15 Co1 O17 95.5(4) . . ?
O15 Co1 O18 95.9(4) 2_655 . ?
O15 Co1 O18 174.9(4) . . ?
O15 Co1 O19 88.2(4) . . ?
O15 Co1 O19 89.2(4) 2_655 . ?
O16 Co1 Co1 87.1(3) . 2_655 ?
O16 Co1 Mo1 136.0(3) . . ?
O16 Co1 Mo5 41.5(3) . . ?
O16 Co1 O17 95.6(4) . . ?
O16 Co1 O18 87.2(4) . . ?
O16 Co1 O19 174.7(4) . . ?
O17 Co1 Co1 137.1(3) . 2_655 ?
O17 Co1 Mo1 127.5(3) . . ?
O17 Co1 Mo5 86.2(3) . . ?
O17 Co1 O18 85.8(4) . . ?
O18 Co1 Co1 137.1(3) . 2_655 ?
O18 Co1 Mo1 87.8(3) . . ?
O18 Co1 Mo5 126.6(3) . . ?
O19 Co1 Co1 87.6(3) . 2_655 ?
O19 Co1 Mo1 41.0(3) . . ?
O19 Co1 Mo5 135.7(3) . . ?
O19 Co1 O17 88.3(4) . . ?
O19 Co1 O18 96.7(4) . . ?
O1 Mo1 Co1 85.3(4) . . ?
O1 Mo1 O3 105.8(5) . . ?
O1 Mo1 O15 88.7(4) . 2_655 ?
O1 Mo1 O19 97.6(4) . . ?
O1 Mo1 O19 157.7(4) . 2_655 ?
O2 Mo1 Co1 132.7(4) . . ?
O2 Mo1 O1 104.0(6) . . ?
O2 Mo1 O3 99.9(5) . . ?
O2 Mo1 O15 164.6(4) . 2_655 ?
O2 Mo1 O19 97.5(5) . 2_655 ?
O2 Mo1 O19 94.4(4) . . ?
O3 Mo1 Co1 122.3(3) . . ?
O3 Mo1 O15 84.5(4) . 2_655 ?
O3 Mo1 O19 148.5(4) . . ?
O3 Mo1 O19 75.3(4) . 2_655 ?
O15 Mo1 Co1 38.5(2) 2_655 . ?
O19 Mo1 Co1 75.9(2) 2_655 . ?
O19 Mo1 Co1 38.4(3) . . ?
O19 Mo1 O15 75.1(3) . 2_655 ?
O19 Mo1 O15 69.1(3) 2_655 2_655 ?
O19 Mo1 O19 75.1(4) . 2_655 ?
O3 Mo2 O6 150.9(4) . . ?
O3 Mo2 O17 82.1(4) . 2_655 ?
O3 Mo2 O19 73.3(3) . 2_655 ?
O4 Mo2 O3 100.5(5) . . ?
O4 Mo2 O6 97.6(5) . . ?
O4 Mo2 O17 160.7(5) . 2_655 ?
O4 Mo2 O19 91.6(5) . 2_655 ?
O5 Mo2 O3 96.9(4) . . ?
O5 Mo2 O4 103.6(6) . . ?
O5 Mo2 O6 100.8(5) . . ?
O5 Mo2 O17 95.1(5) . 2_655 ?
O5 Mo2 O19 163.4(4) . 2_655 ?
O6 Mo2 O17 73.6(4) . 2_655 ?
O6 Mo2 O19 83.6(3) . 2_655 ?
O17 Mo2 O19 70.6(3) 2_655 2_655 ?
O6 Mo3 O9 148.9(4) . . ?
O6 Mo3 O17 72.1(4) . 2_655 ?
O6 Mo3 O18 83.5(4) . 2_655 ?
O7 Mo3 O6 101.3(5) . . ?
O7 Mo3 O9 98.0(5) . . ?
O7 Mo3 O17 90.6(4) . 2_655 ?
O7 Mo3 O18 158.1(4) . 2_655 ?
O8 Mo3 O6 98.3(5) . . ?
O8 Mo3 O7 105.3(5) . . ?
O8 Mo3 O9 99.8(5) . . ?
O8 Mo3 O17 162.9(5) . 2_655 ?
O8 Mo3 O18 94.9(4) . 2_655 ?
O9 Mo3 O17 83.6(4) . 2_655 ?
O9 Mo3 O18 69.9(3) . 2_655 ?
O18 Mo3 O17 70.4(3) 2_655 2_655 ?
O9 Mo4 O16 82.0(4) . 2_655 ?
O9 Mo4 O18 71.2(4) . 2_655 ?
O10 Mo4 O9 101.6(4) . . ?
O10 Mo4 O11 106.3(5) . . ?
O10 Mo4 O12 97.5(4) . . ?
O10 Mo4 O16 162.2(5) . 2_655 ?
O10 Mo4 O18 94.8(5) . 2_655 ?
O11 Mo4 O9 98.3(4) . . ?
O11 Mo4 O12 101.1(4) . . ?
O11 Mo4 O16 90.2(4) . 2_655 ?
O11 Mo4 O18 158.1(4) . 2_655 ?
O12 Mo4 O9 147.6(4) . . ?
O12 Mo4 O16 72.3(3) . 2_655 ?
O12 Mo4 O18 81.5(4) . 2_655 ?
O18 Mo4 O16 69.7(3) 2_655 2_655 ?
O12 Mo5 Co1 122.3(3) . . ?
O12 Mo5 O15 84.0(4) . . ?
O12 Mo5 O16 75.6(3) . 2_655 ?
O12 Mo5 O16 148.2(4) . . ?
O13 Mo5 Co1 132.7(3) . . ?
O13 Mo5 O12 99.3(4) . . ?
O13 Mo5 O14 106.2(5) . . ?
O13 Mo5 O15 163.2(4) . . ?
O13 Mo5 O16 94.0(4) . . ?
O13 Mo5 O16 95.3(4) . 2_655 ?
O14 Mo5 Co1 87.2(3) . . ?
O14 Mo5 O12 102.6(4) . . ?
O14 Mo5 O15 89.0(4) . . ?
O14 Mo5 O16 101.1(4) . . ?
O14 Mo5 O16 158.4(4) . 2_655 ?
O15 Mo5 Co1 38.9(2) . . ?
O15 Mo5 O16 69.4(3) . 2_655 ?
O16 Mo5 Co1 38.6(3) . . ?
O16 Mo5 Co1 76.2(2) 2_655 . ?
O16 Mo5 O15 75.6(3) . . ?
O16 Mo5 O16 74.5(4) . 2_655 ?
C1 N1 C5 118.4(15) . . ?
C1 N1 Zn1 121.7(11) . . ?
C5 N1 Zn1 119.6(11) . . ?
C6 N2 C7 127.6(13) . . ?
C6 N2 C8 118.1(13) . . ?
C7 N2 C8 114.3(13) . . ?
Mo1 O3 Mo2 117.3(5) . . ?
Mo3 O6 Mo2 117.2(5) . . ?
Mo4 O9 Mo3 118.8(4) . . ?
Mo4 O11 Zn1 149.3(6) . . ?
Mo5 O12 Mo4 118.9(5) . . ?
Co1 O15 Co1 96.9(4) . 2_655 ?
Co1 O15 Mo1 91.2(4) 2_655 2_655 ?
Co1 O15 Mo1 101.4(4) . 2_655 ?
Co1 O15 Mo5 103.1(4) 2_655 . ?
Co1 O15 Mo5 92.4(4) . . ?
Mo5 O15 Mo1 158.9(4) . 2_655 ?
Co1 O16 Mo4 99.4(4) . 2_655 ?
Co1 O16 Mo5 100.4(4) . 2_655 ?
Co1 O16 Mo5 99.9(4) . . ?
Mo5 O16 Mo4 155.7(5) . 2_655 ?
Mo5 O16 Mo4 88.0(3) 2_655 2_655 ?
Mo5 O16 Mo5 102.9(4) . 2_655 ?
Co1 O17 Mo2 102.0(4) . 2_655 ?
Co1 O17 Mo3 101.9(4) . 2_655 ?
Mo2 O17 Mo3 92.3(4) 2_655 2_655 ?
Co1 O18 Mo3 101.9(4) . 2_655 ?
Co1 O18 Mo4 103.7(4) . 2_655 ?
Mo4 O18 Mo3 95.8(3) 2_655 2_655 ?
Co1 O19 Mo1 100.6(4) . . ?
Co1 O19 Mo1 100.9(4) . 2_655 ?
Co1 O19 Mo2 99.1(4) . 2_655 ?
Mo1 O19 Mo1 101.9(3) . 2_655 ?
Mo1 O19 Mo2 154.6(4) . 2_655 ?
Mo1 O19 Mo2 89.9(3) 2_655 2_655 ?
N1 Zn1 O11 87.2(5) . . ?
N1 Zn1 O23 177.9(6) . . ?
N1 Zn1 O25 93.7(6) . . ?
O22 Zn1 N1 97.1(6) . . ?
O22 Zn1 O11 90.4(5) . . ?
O22 Zn1 O23 81.1(7) . . ?
O22 Zn1 O25 87.7(6) . . ?
O23 Zn1 O11 91.7(6) . . ?
O24 Zn1 N1 99.5(6) . . ?
O24 Zn1 O11 89.5(5) . . ?
O24 Zn1 O22 163.4(7) . . ?
O24 Zn1 O23 82.3(7) . . ?
O24 Zn1 O25 92.2(6) . . ?
O25 Zn1 O11 177.9(6) . . ?
O25 Zn1 O23 87.3(7) . . ?
N3 C9 C10 120.6(15) . . ?
C11 C10 C9 116.0(16) . . ?
C10 C11 C12 123.6(14) . . ?
C11 C12 C14 123.4(13) . . ?
C13 C12 C11 116.1(14) . . ?
C13 C12 C14 120.5(14) . . ?
C12 C13 N3 122.3(14) . . ?
N4 C14 C12 117.3(13) . . ?
O21 C14 C12 117.9(13) . . ?
O21 C14 N4 124.5(15) . . ?
N4 C15 C16 110.6(14) . 7_655 ?
N4 C16 C15 105.7(14) . 7_655 ?
C9 N3 C13 121.2(14) . . ?
C14 N4 C15 126.1(13) . . ?
C14 N4 C16 119.6(13) . . ?
C15 N4 C16 113.4(12) . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 180.1 35.2 H2O
2 0.000 0.500 0.500 180.1 35.2 H2O
3 0.500 0.000 0.000 180.1 35.2 H2O
4 0.500 1.000 0.500 180.1 35.2 H2O
_shelx_fab_file
;
-29 1 9 0.0093 0.1856
-29 1 10 9.2512 0.0595
-29 3 9 4.4726 0.0975
-29 3 10 3.7019 -0.3544
-29 3 11 4.1445 0.0902
-29 3 12 0.1939 -0.4160
-29 3 13 -1.4852 0.0492
-29 5 10 1.1858 -0.7995
-29 5 11 6.3315 -0.0323
-28 0 6 9.1492 0.4220
-28 0 8 -6.1893 -0.2730
-28 2 6 7.4315 0.1753
-28 2 7 2.3878 -0.1253
-28 2 8 -4.1057 -0.3351
-28 2 9 -3.6538 -0.0845
-28 2 10 -7.8586 0.2067
-28 2 11 -1.1879 0.0599
-28 2 12 -1.7081 0.1869
-28 4 6 6.1556 -0.2131
-28 4 7 -0.9814 -0.0463
-28 4 8 2.4668 0.1195
-28 4 9 -10.0237 -0.1654
-28 4 10 -4.0915 0.6886
-28 4 11 -5.4237 -0.1197
-28 4 12 0.5689 0.2716
-28 4 13 3.6155 -0.3973
-28 6 8 6.0764 0.3031
-28 6 9 -2.0517 0.0160
-28 6 10 -0.6838 0.6190
-28 6 11 -5.8650 -0.0070
-28 6 12 -0.1770 0.4346
-27 1 2 10.8865 1.2652
-27 1 3 -3.1180 -0.0283
-27 1 4 -7.4750 0.2351
-27 1 5 -3.0849 0.0285
-27 1 6 -4.8798 -0.3439
-27 1 7 -1.7094 0.2496
-27 1 8 8.8900 0.3727
-27 1 9 0.9290 0.0093
-27 1 10 10.1253 -0.1967
-27 1 11 -0.9384 -0.1664
-27 1 12 5.0423 0.0581
-27 1 13 -0.0492 -0.0534
-27 3 3 -3.5441 0.0624
-27 3 4 -5.7498 0.0041
-27 3 5 -4.8435 -0.1500
-27 3 6 -3.6499 0.0578
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26 2 2 -5.5879 -0.1473
26 2 3 3.7866 -0.2098
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0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
1.res created by SHELXL-2014/7
TITL 1_a.res in C2/c
REM Old TITL 1 in C2/c
REM SHELXT solution in C2/c
REM R1 0.195, Rweak 0.011, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C21 N5 O21 Zn Mo6
CELL 0.71073 21.5443 14.2328 24.2463 90 104.817 90
ZERR 4 0.002 0.0012 0.0027 0 0.01 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Co Mo N O Zn
UNIT 128 176 8 40 32 200 8
ISOR 0.001 0.002 O13
ISOR 0.001 0.002 O11
ISOR 0.001 0.002 O19
ISOR 0.001 0.002 O25
L.S. 30 0 0
PLAN 5
list 4
ABIN
omit-2 52
fmap 2 53
acta
OMIT -9 7 8
OMIT -6 2 9
REM
REM
REM
WGHT 0.045600 642.203125
FVAR 0.06910
C1 1 0.672837 0.160911 0.496357 11.00000 0.03263 0.06462 =
0.05467 0.01021 0.01272 0.01688
AFIX 43
H1 2 0.709900 0.128947 0.494507 11.00000 -1.20000
AFIX 0
C2 1 0.670032 0.200773 0.546969 11.00000 0.04933 0.10065 =
0.04211 -0.00151 -0.00356 0.03831
AFIX 43
H2 2 0.703242 0.191184 0.579529 11.00000 -1.20000
AFIX 0
C3 1 0.618103 0.255045 0.549726 11.00000 0.03337 0.06696 =
0.04275 -0.01880 -0.00486 0.00794
AFIX 43
H3 2 0.616994 0.286520 0.583074 11.00000 -1.20000
AFIX 0
C4 1 0.567768 0.261397 0.501608 11.00000 0.03318 0.03633 =
0.03805 0.02078 0.00740 0.00034
C5 1 0.573308 0.216399 0.452923 11.00000 0.03355 0.05438 =
0.04042 0.02307 0.01244 0.00687
AFIX 43
H5 2 0.539626 0.220913 0.420228 11.00000 -1.20000
AFIX 0
C6 1 0.505318 0.311487 0.500821 11.00000 0.04126 0.04070 =
0.03478 0.01595 0.00810 -0.00460
C7 1 0.564034 0.464643 0.521921 11.00000 0.02357 0.04296 =
0.04038 -0.00112 0.00311 0.00246
AFIX 23
H7A 2 0.600236 0.429383 0.515829 11.00000 -1.20000
H7B 2 0.575048 0.486459 0.561124 11.00000 -1.20000
AFIX 0
C8 1 0.448943 0.451818 0.517956 11.00000 0.04042 0.03520 =
0.04410 0.00364 0.01843 0.00927
AFIX 23
H8A 2 0.454234 0.472573 0.556992 11.00000 -1.20000
H8B 2 0.413009 0.408528 0.508388 11.00000 -1.20000
AFIX 0
CO1 3 0.433322 0.537551 0.232113 11.00000 0.01642 0.01405 =
0.01995 0.00096 0.00750 0.00228
MO1 4 0.491141 0.694551 0.179725 11.00000 0.03081 0.02447 =
0.02748 0.00321 0.01290 -0.00259
MO2 4 0.647536 0.699935 0.224427 11.00000 0.02870 0.03138 =
0.03749 0.00149 0.01475 -0.01143
MO3 4 0.724520 0.536911 0.311820 11.00000 0.01941 0.03191 =
0.03001 -0.00693 0.00972 -0.00746
MO4 4 0.639233 0.374372 0.357447 11.00000 0.01719 0.02787 =
0.02359 0.00200 0.00606 0.00400
MO5 4 0.482659 0.384551 0.313359 11.00000 0.01704 0.01917 =
0.02334 0.00336 0.00732 -0.00004
N1 5 0.625487 0.166078 0.450641 11.00000 0.03730 0.04017 =
0.03205 0.01092 0.01104 0.01065
N2 5 0.508277 0.404092 0.512281 11.00000 0.02153 0.04056 =
0.05080 -0.00214 0.01475 0.00384
O1 6 0.434773 0.666871 0.118201 11.00000 0.03879 0.03744 =
0.04419 0.00574 0.01438 0.00691
O2 6 0.486407 0.814096 0.184083 11.00000 0.06330 0.04655 =
0.03889 0.00672 0.02641 -0.00186
O3 6 0.571509 0.683145 0.162411 11.00000 0.02316 0.03886 =
0.03451 0.00117 0.01194 -0.00018
O4 6 0.643499 0.819234 0.236236 11.00000 0.03736 0.05637 =
0.05761 0.00195 0.00932 -0.00684
O5 6 0.702108 0.691483 0.184621 11.00000 0.04248 0.04776 =
0.03358 -0.00199 0.00609 -0.01489
O6 6 0.700445 0.666033 0.299298 11.00000 0.03492 0.03226 =
0.02233 -0.00523 0.01331 -0.02224
O7 6 0.774835 0.523809 0.268273 11.00000 0.02605 0.04570 =
0.05304 -0.01731 0.01762 -0.01167
O8 6 0.772745 0.547231 0.377909 11.00000 0.03374 0.06820 =
0.03777 -0.02700 0.00352 -0.01833
O9 6 0.699141 0.407366 0.313762 11.00000 0.02756 0.02788 =
0.02686 -0.01194 0.01462 0.00033
O10 6 0.685463 0.384964 0.425227 11.00000 0.02049 0.05269 =
0.02977 0.00245 -0.00071 -0.00362
O11 6 0.633840 0.256843 0.342766 11.00000 0.03256 0.03196 =
0.03259 0.00060 0.00823 0.00057
O12 6 0.558461 0.397319 0.373165 11.00000 0.02146 0.02807 =
0.02024 0.01179 0.00749 0.00843
O13 6 0.480890 0.265744 0.306804 11.00000 0.02640 0.02292 =
0.02753 0.00135 0.00705 -0.00041
O14 6 0.423909 0.413019 0.346070 11.00000 0.03178 0.03276 =
0.02667 0.00978 0.01412 0.00270
O15 6 0.496744 0.536307 0.299961 11.00000 0.02252 0.02983 =
0.01414 -0.00964 0.00903 0.00257
O16 6 0.437847 0.406488 0.232312 11.00000 0.02309 0.02160 =
0.03258 0.00633 0.00767 0.00243
O17 6 0.363403 0.544624 0.266844 11.00000 0.01861 0.03927 =
0.03058 -0.00358 0.01690 0.00440
O18 6 0.367076 0.526847 0.159292 11.00000 0.01879 0.02013 =
0.02490 0.00968 0.00815 0.00624
O19 6 0.437138 0.670283 0.234109 11.00000 0.01999 0.01923 =
0.02005 -0.00016 0.00546 0.00062
O20 6 0.455301 0.267005 0.490138 11.00000 0.02844 0.04731 =
0.07048 -0.00725 0.00558 -0.00831
O22 6 0.537289 0.101906 0.335851 11.00000 0.06017 0.04525 =
0.10498 -0.00480 -0.01258 0.00258
AFIX 7
H22A 2 0.528731 0.085415 0.298769 11.00000 -1.50000
H22B 2 0.517007 0.157944 0.333715 11.00000 -1.50000
AFIX 0
O23 6 0.636761 0.056005 0.291710 11.00000 0.08166 0.09547 =
0.13052 -0.01157 0.05058 0.01146
AFIX 7
H23A 2 0.600150 0.021769 0.273296 11.00000 -1.50000
H23B 2 0.668433 0.009813 0.293194 11.00000 -1.50000
AFIX 0
O24 6 0.728698 0.105836 0.387475 11.00000 0.04833 0.05175 =
0.11488 0.03932 0.04610 0.03179
AFIX 7
H24A 2 0.741954 0.105812 0.355158 11.00000 -1.50000
H24B 2 0.745282 0.051497 0.403559 11.00000 -1.50000
AFIX 0
O25 6 0.628265 -0.030667 0.399609 11.00000 0.08896 0.08886 =
0.08990 0.00192 0.02309 0.00098
ZN1 7 0.632619 0.110532 0.372938 11.00000 0.03798 0.04320 =
0.05576 0.01413 0.02256 0.01550
C9 1 0.660707 0.237833 0.212010 11.00000 0.03197 0.05696 =
0.04418 0.01364 0.01973 0.02132
AFIX 43
H9 2 0.648345 0.211845 0.242752 11.00000 -1.20000
AFIX 0
C10 1 0.639853 0.197033 0.158114 11.00000 0.03540 0.03744 =
0.03678 0.00168 0.01279 0.00865
AFIX 43
H10 2 0.614222 0.143534 0.151835 11.00000 -1.20000
AFIX 0
C11 1 0.659213 0.240105 0.115328 11.00000 0.03133 0.04523 =
0.02820 -0.01742 0.00179 0.00723
AFIX 43
H11 2 0.644511 0.216402 0.078549 11.00000 -1.20000
AFIX 0
C12 1 0.699745 0.317568 0.123515 11.00000 0.01617 0.03581 =
0.02678 0.00136 0.00418 0.00649
C13 1 0.718686 0.350348 0.176943 11.00000 0.02848 0.04045 =
0.03815 -0.01748 0.00459 -0.01167
AFIX 43
H13 2 0.747211 0.400582 0.184556 11.00000 -1.20000
AFIX 0
C14 1 0.719956 0.365037 0.076678 11.00000 0.03042 0.02555 =
0.04005 -0.00157 0.01086 0.00777
C15 1 0.774877 0.220599 0.056964 11.00000 0.06246 0.04164 =
0.03870 0.00093 0.02865 0.01439
AFIX 23
H15A 2 0.768705 0.199558 0.093242 11.00000 -1.20000
H15B 2 0.820657 0.226074 0.060762 11.00000 -1.20000
AFIX 0
C16 1 0.753693 0.351093 -0.010953 11.00000 0.07370 0.02603 =
0.03895 0.00493 0.03113 0.01846
AFIX 23
H16A 2 0.798958 0.360428 -0.008320 11.00000 -1.20000
H16B 2 0.731766 0.410942 -0.019318 11.00000 -1.20000
AFIX 0
N3 5 0.698012 0.313364 0.219797 11.00000 0.03808 0.04774 =
0.02615 0.01300 0.00880 0.02736
N4 5 0.744635 0.311623 0.042693 11.00000 0.05478 0.03254 =
0.03422 0.00090 0.02146 0.01059
O21 6 0.707649 0.447888 0.068909 11.00000 0.04834 0.03524 =
0.03800 -0.00758 0.01012 -0.00013
HKLF 4
REM 1_a.res in C2/c
REM R1 = 0.0921 for 5513 Fo > 4sig(Fo) and 0.1109 for all 7033 data
REM 472 parameters refined using 24 restraints
END
WGHT 0.0443 641.3291
REM Highest difference peak 3.009, deepest hole -2.305, 1-sigma level 0.272
Q1 1 0.6411 -0.1603 0.3458 11.00000 0.05 3.01
Q2 1 0.6461 0.7590 0.2234 11.00000 0.05 1.81
Q3 1 0.5303 -0.0266 0.2326 11.00000 0.05 1.71
Q4 1 0.4977 0.7597 0.1775 11.00000 0.05 1.62
Q5 1 0.5626 0.1082 0.3001 11.00000 0.05 1.45
REM The information below was added by Olex2.
REM
REM R1 = 0.0921 for 5513 Fo > 4sig(Fo) and 0.1109 for all 20887 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 3.01, deepest hole -2.31
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.1109
REM R1_gt = 0.0921
REM wR_ref = 0.2129
REM GOOF = 1.091
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 20887
REM Reflections_gt = 5513
REM Parameters = n/a
REM Hole = -2.31
REM Peak = 3.01
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'