# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1540180'
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_audit_creation_date 2017-09-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'Cr H5 Mo6 O24, 2.5(C8.8 H8.4 N2.4 O0.8), 0.5(H4 O2)'
_chemical_formula_sum 'C22 H28 Cr Mo6 N6 O27'
_chemical_formula_weight 1436.14
_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'
Cr Cr 0.3209 0.6236 '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 6.0210(5)
_cell_length_b 12.3200(9)
_cell_length_c 13.2940(10)
_cell_angle_alpha 77.8710(10)
_cell_angle_beta 77.2590(10)
_cell_angle_gamma 79.4860(10)
_cell_volume 930.75(12)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 3571
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.253
_cell_measurement_theta_min 1.51
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.347
_exptl_absorpt_correction_T_max 0.889
_exptl_absorpt_correction_T_min 0.798
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.562
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 694
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0142
_diffrn_reflns_av_unetI/netI 0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 6844
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full 25.240
_diffrn_reflns_theta_max 28.253
_diffrn_reflns_theta_min 1.596
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4048
_reflns_number_total 4541
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_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 'Bruker SHELXTL'
_refine_diff_density_max 0.468
_refine_diff_density_min -0.512
_refine_diff_density_rms 0.097
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 4541
_refine_ls_number_restraints 256
_refine_ls_R_factor_all 0.0275
_refine_ls_R_factor_gt 0.0230
_refine_ls_restrained_S_all 1.019
_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^)+(0.0290P)^2^+0.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0538
_refine_ls_wR_factor_ref 0.0559
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups, All O(H) groups
At 1.5 times of:
All O(H,H) groups
2. Restrained distances
O1-C6 \\sim O1A-C6A
with sigma of 0.02
N1-C1 \\sim N1A-C1A
with sigma of 0.02
N1-C2 \\sim N1A-C2A
with sigma of 0.02
C1-C5 \\sim C1A-C5A
with sigma of 0.02
N2-C5 \\sim N2A-C5A
with sigma of 0.02
N2-C6 \\sim N2A-C6A
with sigma of 0.02
C2-C3 \\sim C2A-C3A
with sigma of 0.02
C3-C4 \\sim C3A-C4A
with sigma of 0.02
N3-C11 \\sim N3A-C8A
with sigma of 0.02
N3-C10 \\sim N3A-C9A
with sigma of 0.02
C4-C5 \\sim C4A-C5A
with sigma of 0.02
C6-C7 \\sim C6A-C7A
with sigma of 0.02
C7-C11 \\sim C7A-C8A
with sigma of 0.02
C7-C8 \\sim C7A-C11A
with sigma of 0.02
C9-C10 \\sim C10A-C9A
with sigma of 0.02
C9-C8 \\sim C10A-C11A
with sigma of 0.02
O1-N2 \\sim O1A-N2A
with sigma of 0.04
O1-C7 \\sim O1A-C7A
with sigma of 0.04
N1-C3 \\sim N1A-C3A
with sigma of 0.04
N1-C5 \\sim N1A-C5A
with sigma of 0.04
C1-N2 \\sim C1A-N2A
with sigma of 0.04
C1-C2 \\sim C1A-C2A
with sigma of 0.04
C1-C4 \\sim C1A-C4A
with sigma of 0.04
N2-C4 \\sim N2A-C4A
with sigma of 0.04
N2-C7 \\sim N2A-C7A
with sigma of 0.04
C2-C4 \\sim C2A-C4A
with sigma of 0.04
C3-C5 \\sim C3A-C5A
with sigma of 0.04
N3-C7 \\sim N3A-C7A
with sigma of 0.04
N3-C9 \\sim N3A-C10A
with sigma of 0.04
C5-C6 \\sim C5A-C6A
with sigma of 0.04
C6-C11 \\sim C6A-C8A
with sigma of 0.04
C6-C8 \\sim C6A-C11A
with sigma of 0.04
C7-C9 \\sim C7A-C10A
with sigma of 0.04
C11-C10 \\sim C8A-C9A
with sigma of 0.04
C11-C8 \\sim C8A-C11A
with sigma of 0.04
C10-C8 \\sim C9A-C11A
with sigma of 0.04
3. Rigid bond restraints
C6, C7
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Rigid body (RIGU) restrains
O1A, N1A, N2A, N3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
O1, N1, N2, N3, C1, C11, C2, C3, C4, C5, C6, C7, C8, C9, C10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Fixed Sof: H8B(0.5) O1(0.8) N1(0.8) H1(0.8) N2(0.8) H2(0.8) N3(0.8) H3(0.4)
C1(0.8) H1A(0.8) C11(0.8) H11(0.8) C2(0.8) H2A(0.8) C3(0.8) H3A(0.8) C4(0.8)
H4(0.8) C5(0.8) C6(0.8) C7(0.8) C8(0.8) H8(0.8) C9(0.8) H9(0.8) C10(0.8)
H10(0.8) O1A(0.2) N1A(0.2) H1AC(0.15) N2A(0.2) H2AA(0.2) N3A(0.2) H3AA(0.15)
C1A(0.2) H1AB(0.2) C2A(0.2) H2AB(0.2) C3A(0.2) H3AB(0.2) C4A(0.2) H4A(0.2)
C5A(0.2) C6A(0.2) C7A(0.2) C8A(0.2) H8A(0.2) C9A(0.2) H9A(0.2) C10A(0.2)
H10A(0.2) C11A(0.2) H11A(0.2) H1WA(0.5) H1WB(0.5)
6.a Free rotating group:
O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
O4(H4B), O8(H8B), O9(H9B)
6.c Aromatic/amide H refined with riding coordinates:
N1(H1), N2(H2), N3(H3), C1(H1A), C11(H11), C2(H2A), C3(H3A), C4(H4), C8(H8),
C9(H9), C10(H10), N1A(H1AC), N2A(H2AA), N3A(H3AA), C1A(H1AB), C2A(H2AB),
C3A(H3AB), C4A(H4A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.56363(4) 0.62751(2) -0.25010(2) 0.01900(6) Uani 1 1 d . . . . .
Mo2 Mo 0.67378(3) 0.60681(2) 0.17291(2) 0.01920(6) Uani 1 1 d . . . . .
Mo3 Mo 0.72828(3) 0.73471(2) -0.07282(2) 0.01853(6) Uani 1 1 d . . . . .
Cr1 Cr 0.5000 0.5000 0.0000 0.01344(10) Uani 1 2 d S T P . .
O2 O 0.9423(3) 0.63150(15) 0.17784(15) 0.0275(4) Uani 1 1 d . . . . .
O3 O 0.5795(3) 0.73966(14) 0.07263(14) 0.0223(4) Uani 1 1 d . . . . .
O4 O 0.3744(3) 0.53717(13) 0.14046(13) 0.0162(3) Uani 1 1 d . . . . .
H4B H 0.2211 0.5814 0.1518 0.019 Uiso 1 1 calc R . . . .
O5 O 1.0002(3) 0.75780(15) -0.07128(15) 0.0251(4) Uani 1 1 d . . . . .
O6 O 0.4945(3) 0.65826(16) 0.27615(15) 0.0287(4) Uani 1 1 d . . . . .
O7 O 0.5911(3) 0.86171(15) -0.12005(16) 0.0295(4) Uani 1 1 d . . . . .
O8 O 0.2266(3) 0.44021(13) -0.01583(13) 0.0175(3) Uani 1 1 d . . . . .
H8B H 0.0762 0.4857 0.0004 0.021 Uiso 0.5 1 calc R . . A -1
O9 O 0.4274(3) 0.65140(13) -0.08103(13) 0.0166(3) Uani 1 1 d . . . . .
H9B H 0.2718 0.6917 -0.0638 0.020 Uiso 1 1 calc R . . . .
O10 O 0.8095(3) 0.66691(15) -0.19857(14) 0.0252(4) Uani 1 1 d . . . . .
O11 O 0.4322(4) 0.75635(15) -0.30044(16) 0.0341(5) Uani 1 1 d . . . . .
O12 O 0.7274(4) 0.57278(17) -0.35432(15) 0.0353(5) Uani 1 1 d . . . . .
O13 O 0.2917(3) 0.55219(14) -0.22687(15) 0.0251(4) Uani 1 1 d . . . . .
O1 O 0.6876(16) 0.9924(7) -0.3988(9) 0.0443(15) Uani 0.8 1 d D U . B 1
N1 N 0.7794(7) 1.1285(5) -0.1573(6) 0.0241(10) Uani 0.8 1 d D U . B 1
H1 H 0.6548 1.1726 -0.1399 0.029 Uiso 0.8 1 calc R . . B 1
N2 N 1.0040(5) 0.9194(2) -0.3283(2) 0.0260(6) Uani 0.8 1 d D U . B 1
H2 H 1.1227 0.8685 -0.3320 0.031 Uiso 0.8 1 calc R . . B 1
N3 N 1.1323(8) 0.6688(4) -0.5164(4) 0.0433(12) Uani 0.8 1 d D U . B 1
H3 H 1.2490 0.6171 -0.5129 0.052 Uiso 0.4 1 calc R . . B 1
C1 C 0.7908(10) 1.0677(5) -0.2326(6) 0.0301(13) Uani 0.8 1 d D U . B 1
H1A H 0.6689 1.0772 -0.2676 0.036 Uiso 0.8 1 calc R . . B 1
C11 C 1.0932(8) 0.7474(4) -0.4558(4) 0.0418(12) Uani 0.8 1 d D U . B 1
H11 H 1.1934 0.7449 -0.4110 0.050 Uiso 0.8 1 calc R . . B 1
C2 C 0.9550(8) 1.1221(5) -0.1091(5) 0.0276(11) Uani 0.8 1 d D U . B 1
H2A H 0.9434 1.1672 -0.0596 0.033 Uiso 0.8 1 calc R . . B 1
C3 C 1.1534(8) 1.0489(4) -0.1326(4) 0.0305(10) Uani 0.8 1 d D U . B 1
H3A H 1.2759 1.0436 -0.0989 0.037 Uiso 0.8 1 calc R . . B 1
C4 C 1.1674(7) 0.9830(4) -0.2075(4) 0.0261(9) Uani 0.8 1 d D U . B 1
H4 H 1.3001 0.9331 -0.2241 0.031 Uiso 0.8 1 calc R . . B 1
C5 C 0.9854(7) 0.9914(3) -0.2573(4) 0.0212(9) Uani 0.8 1 d D U . B 1
C6 C 0.8553(6) 0.9211(3) -0.3919(3) 0.0267(7) Uani 0.8 1 d D U . B 1
C7 C 0.9089(7) 0.8315(4) -0.4583(3) 0.0247(9) Uani 0.8 1 d D U . B 1
C8 C 0.7588(11) 0.8312(5) -0.5235(5) 0.0321(12) Uani 0.8 1 d D U . B 1
H8 H 0.6264 0.8835 -0.5244 0.038 Uiso 0.8 1 calc R . . B 1
C9 C 0.8117(16) 0.7491(9) -0.5888(8) 0.046(2) Uani 0.8 1 d D U . B 1
H9 H 0.7203 0.7498 -0.6370 0.055 Uiso 0.8 1 calc R . . B 1
C10 C 0.9965(12) 0.6698(6) -0.5801(6) 0.0412(15) Uani 0.8 1 d D U . B 1
H10 H 1.0276 0.6142 -0.6209 0.049 Uiso 0.8 1 calc R . . B 1
O1A O 0.698(7) 1.011(3) -0.393(4) 0.041(5) Uani 0.2 1 d D U . C 2
N1A N 0.772(4) 0.758(2) -0.573(2) 0.024(3) Uani 0.2 1 d D U . C 2
H1AC H 0.6512 0.7676 -0.5998 0.029 Uiso 0.15 1 calc R . . C 2
N2A N 0.996(2) 0.8665(9) -0.3813(9) 0.030(2) Uani 0.2 1 d D U . C 2
H2AA H 1.1097 0.8423 -0.3496 0.036 Uiso 0.2 1 calc R . . C 2
N3A N 1.163(3) 1.0314(17) -0.1603(15) 0.035(4) Uani 0.2 1 d D U . C 2
H3AA H 1.2932 1.0136 -0.1405 0.042 Uiso 0.15 1 calc R . . C 2
C1A C 0.798(5) 0.829(2) -0.511(3) 0.035(5) Uani 0.2 1 d D U . C 2
H1AB H 0.6967 0.8956 -0.5068 0.042 Uiso 0.2 1 calc R . . C 2
C2A C 0.943(5) 0.672(3) -0.589(3) 0.034(5) Uani 0.2 1 d D U . C 2
H2AB H 0.9399 0.6292 -0.6389 0.041 Uiso 0.2 1 calc R . . C 2
C3A C 1.117(4) 0.6461(19) -0.536(2) 0.037(4) Uani 0.2 1 d D U . C 2
H3AB H 1.2253 0.5826 -0.5438 0.044 Uiso 0.2 1 calc R . . C 2
C4A C 1.134(3) 0.7135(16) -0.4708(18) 0.037(4) Uani 0.2 1 d D U . C 2
H4A H 1.2584 0.6977 -0.4367 0.044 Uiso 0.2 1 calc R . . C 2
C5A C 0.974(3) 0.8036(14) -0.4538(14) 0.026(3) Uani 0.2 1 d D U . C 2
C6A C 0.861(2) 0.9602(10) -0.3547(10) 0.023(2) Uani 0.2 1 d D U . C 2
C7A C 0.921(3) 1.0092(15) -0.2704(14) 0.021(3) Uani 0.2 1 d D U . C 2
C8A C 1.119(3) 0.9800(16) -0.2332(15) 0.027(3) Uani 0.2 1 d D U . C 2
H8A H 1.2276 0.9232 -0.2582 0.033 Uiso 0.2 1 calc R . . C 2
C9A C 1.009(4) 1.107(2) -0.120(2) 0.028(4) Uani 0.2 1 d D U . C 2
H9A H 1.0304 1.1367 -0.0646 0.033 Uiso 0.2 1 calc R . . C 2
C10A C 0.821(3) 1.142(3) -0.161(3) 0.026(5) Uani 0.2 1 d D U . C 2
H10A H 0.7274 1.2062 -0.1426 0.031 Uiso 0.2 1 calc R . . C 2
C11A C 0.754(4) 1.088(2) -0.229(2) 0.026(4) Uani 0.2 1 d D U . C 2
H11A H 0.6082 1.1042 -0.2460 0.031 Uiso 0.2 1 calc R . . C 2
O1W O 1.5000 0.5000 -0.5000 0.0960(19) Uani 1 2 d S T P . .
H1WA H 1.4348 0.4733 -0.5380 0.144 Uiso 0.5 1 d G . . . .
H1WB H 1.5266 0.4501 -0.4476 0.144 Uiso 0.5 1 d G . . . .
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
Mo1 0.02173(11) 0.01841(11) 0.01715(11) -0.00307(8) -0.00514(8) -0.00193(8)
Mo2 0.01366(10) 0.02365(11) 0.02402(12) -0.01246(8) -0.00544(8) -0.00038(8)
Mo3 0.01268(10) 0.01516(10) 0.02859(12) -0.00494(8) -0.00501(8) -0.00153(7)
Cr1 0.0104(2) 0.0149(2) 0.0155(3) -0.00367(19) -0.00348(19) -0.00066(18)
O2 0.0184(9) 0.0313(10) 0.0369(11) -0.0119(8) -0.0109(8) 0.0000(7)
O3 0.0180(8) 0.0220(9) 0.0265(10) -0.0082(7) -0.0045(7) 0.0028(7)
O4 0.0120(7) 0.0194(8) 0.0179(8) -0.0062(6) -0.0031(6) -0.0003(6)
O5 0.0168(8) 0.0245(9) 0.0358(11) -0.0081(8) -0.0058(8) -0.0029(7)
O6 0.0270(10) 0.0331(10) 0.0274(10) -0.0142(8) -0.0025(8) -0.0012(8)
O7 0.0259(9) 0.0225(9) 0.0384(12) -0.0010(8) -0.0096(8) 0.0000(7)
O8 0.0117(7) 0.0199(8) 0.0222(9) -0.0061(7) -0.0044(6) -0.0018(6)
O9 0.0129(7) 0.0154(8) 0.0216(9) -0.0046(6) -0.0043(6) 0.0007(6)
O10 0.0248(9) 0.0268(9) 0.0249(10) -0.0090(7) 0.0013(8) -0.0082(7)
O11 0.0495(12) 0.0219(9) 0.0303(11) -0.0012(8) -0.0143(9) 0.0013(9)
O12 0.0486(12) 0.0309(10) 0.0236(11) -0.0075(8) 0.0011(9) -0.0046(9)
O13 0.0287(9) 0.0210(9) 0.0295(10) -0.0047(7) -0.0167(8) 0.0002(7)
O1 0.044(2) 0.043(3) 0.056(3) -0.028(2) -0.031(2) 0.017(2)
N1 0.0175(16) 0.0192(19) 0.0357(19) -0.0105(14) -0.0026(16) 0.0006(15)
N2 0.0259(14) 0.0256(14) 0.0279(15) -0.0122(11) -0.0101(12) 0.0072(11)
N3 0.0338(19) 0.049(3) 0.051(3) -0.030(2) -0.0068(18) 0.0060(17)
C1 0.025(2) 0.029(3) 0.039(3) -0.014(2) -0.010(2) 0.0035(18)
C11 0.034(2) 0.050(3) 0.050(3) -0.033(2) -0.017(2) 0.009(2)
C2 0.024(2) 0.025(2) 0.036(2) -0.0192(18) -0.0041(19) 0.0060(17)
C3 0.031(2) 0.029(2) 0.035(3) -0.0171(18) -0.0106(18) 0.0030(17)
C4 0.0237(19) 0.0254(18) 0.031(2) -0.0130(16) -0.0069(15) 0.0028(14)
C5 0.023(2) 0.0159(17) 0.0241(19) -0.0039(14) -0.0055(15) 0.0001(14)
C6 0.0291(17) 0.0269(17) 0.0261(18) -0.0083(13) -0.0084(14) -0.0011(13)
C7 0.023(2) 0.028(2) 0.0231(18) -0.0079(15) -0.0041(15) -0.0009(14)
C8 0.037(3) 0.033(2) 0.029(3) -0.0035(18) -0.013(2) -0.0058(19)
C9 0.058(4) 0.052(4) 0.037(4) -0.019(3) -0.018(4) -0.004(3)
C10 0.044(4) 0.045(3) 0.036(3) -0.018(2) -0.002(2) -0.004(2)
O1A 0.050(7) 0.035(7) 0.045(8) -0.024(7) -0.025(7) 0.013(6)
N1A 0.030(5) 0.026(6) 0.016(6) -0.006(4) -0.001(5) -0.003(4)
N2A 0.038(4) 0.026(4) 0.029(4) -0.013(3) -0.012(4) 0.003(3)
N3A 0.034(5) 0.036(7) 0.042(7) -0.025(6) -0.013(5) 0.008(4)
C1A 0.041(6) 0.034(6) 0.035(9) -0.019(6) -0.017(7) 0.007(5)
C2A 0.035(7) 0.035(7) 0.037(8) -0.021(7) -0.013(7) 0.004(5)
C3A 0.040(6) 0.034(5) 0.044(8) -0.024(6) -0.018(6) 0.006(5)
C4A 0.041(5) 0.033(5) 0.043(8) -0.023(5) -0.020(5) 0.008(5)
C5A 0.034(5) 0.023(4) 0.022(5) -0.008(4) -0.007(4) -0.001(4)
C6A 0.029(4) 0.019(3) 0.020(4) -0.004(3) -0.001(3) -0.005(3)
C7A 0.027(4) 0.016(5) 0.019(5) -0.003(4) -0.001(3) -0.005(3)
C8A 0.031(5) 0.025(6) 0.029(6) -0.013(5) -0.006(4) 0.001(4)
C9A 0.029(5) 0.025(6) 0.032(6) -0.015(5) -0.006(5) 0.001(4)
C10A 0.027(6) 0.023(6) 0.029(8) -0.012(6) -0.004(6) -0.001(5)
C11A 0.029(4) 0.023(6) 0.027(6) -0.010(6) -0.003(4) -0.002(4)
O1W 0.123(4) 0.084(3) 0.099(4) -0.041(3) -0.083(4) 0.045(3)
_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
Mo1 O4 2.2586(16) 2_665 y
Mo1 O9 2.2777(17) . y
Mo1 O10 1.9353(18) . y
Mo1 O11 1.7093(18) . y
Mo1 O12 1.701(2) . y
Mo1 O13 1.9617(18) . y
Mo2 O2 1.7162(17) . y
Mo2 O3 1.9637(17) . y
Mo2 O4 2.2882(15) . y
Mo2 O6 1.7069(18) . y
Mo2 O8 2.2102(17) 2_665 y
Mo2 O13 1.9292(17) 2_665 y
Mo3 O3 1.9522(18) . y
Mo3 O5 1.7171(17) . y
Mo3 O7 1.6937(18) . y
Mo3 O8 2.2287(16) 2_665 y
Mo3 O9 2.2715(16) . y
Mo3 O10 1.9515(18) . y
Cr1 O4 1.9693(16) 2_665 y
Cr1 O4 1.9694(16) . y
Cr1 O8 1.9894(15) . y
Cr1 O8 1.9894(15) 2_665 y
Cr1 O9 1.9739(16) 2_665 y
Cr1 O9 1.9739(16) . y
O4 Mo1 2.2586(16) 2_665 y
O8 Mo2 2.2103(17) 2_665 y
O8 Mo3 2.2288(16) 2_665 y
O13 Mo2 1.9292(17) 2_665 y
O1 C6 1.218(5) . ?
N1 C1 1.354(6) . ?
N1 C2 1.335(5) . ?
N2 C5 1.400(4) . ?
N2 C6 1.354(4) . ?
N3 C11 1.342(5) . ?
N3 C10 1.297(6) . ?
C1 C5 1.387(5) . ?
C11 C7 1.374(5) . ?
C2 C3 1.378(5) . ?
C3 C4 1.391(5) . ?
C4 C5 1.378(5) . ?
C6 C7 1.503(5) . ?
C7 C8 1.384(5) . ?
C8 C9 1.417(7) . ?
C9 C10 1.348(8) . ?
O1A C6A 1.215(15) . ?
N1A C1A 1.373(18) . ?
N1A C2A 1.354(18) . ?
N2A C5A 1.398(14) . ?
N2A C6A 1.349(12) . ?
N3A C8A 1.357(15) . ?
N3A C9A 1.302(16) . ?
C1A C5A 1.385(16) . ?
C2A C3A 1.351(17) . ?
C3A C4A 1.347(15) . ?
C4A C5A 1.354(15) . ?
C6A C7A 1.514(14) . ?
C7A C8A 1.349(15) . ?
C7A C11A 1.367(16) . ?
C9A C10A 1.322(19) . ?
C10A C11A 1.396(18) . ?
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
O4 Mo1 O9 70.11(6) 2_665 . y
O10 Mo1 O4 84.22(7) . 2_665 y
O10 Mo1 O9 72.07(6) . . y
O10 Mo1 O13 150.58(8) . . y
O11 Mo1 O4 160.01(8) . 2_665 y
O11 Mo1 O9 93.40(8) . . y
O11 Mo1 O10 101.83(9) . . y
O11 Mo1 O13 95.19(9) . . y
O12 Mo1 O4 91.60(8) . 2_665 y
O12 Mo1 O9 159.62(8) . . y
O12 Mo1 O10 97.91(9) . . y
O12 Mo1 O11 106.20(10) . . y
O12 Mo1 O13 100.15(9) . . y
O13 Mo1 O4 72.29(6) . 2_665 y
O13 Mo1 O9 83.21(7) . . y
O2 Mo2 O3 100.30(8) . . y
O2 Mo2 O4 164.09(7) . . y
O2 Mo2 O8 95.42(8) . 2_665 y
O2 Mo2 O13 98.71(8) . 2_665 y
O3 Mo2 O4 84.62(7) . . y
O3 Mo2 O8 73.08(6) . 2_665 y
O6 Mo2 O2 105.15(9) . . y
O6 Mo2 O3 92.18(8) . . y
O6 Mo2 O4 89.66(8) . . y
O6 Mo2 O8 156.66(8) . 2_665 y
O6 Mo2 O13 101.37(9) . 2_665 y
O8 Mo2 O4 71.38(6) 2_665 . y
O13 Mo2 O3 152.85(7) 2_665 . y
O13 Mo2 O4 72.17(6) 2_665 . y
O13 Mo2 O8 86.01(7) 2_665 2_665 y
O3 Mo3 O8 72.86(6) . 2_665 y
O3 Mo3 O9 85.76(7) . . y
O5 Mo3 O3 100.80(8) . . y
O5 Mo3 O8 94.28(7) . 2_665 y
O5 Mo3 O9 162.45(7) . . y
O5 Mo3 O10 96.86(8) . . y
O7 Mo3 O3 94.24(9) . . y
O7 Mo3 O5 105.08(9) . . y
O7 Mo3 O8 158.59(8) . 2_665 y
O7 Mo3 O9 90.50(8) . . y
O7 Mo3 O10 100.43(9) . . y
O8 Mo3 O9 71.93(6) 2_665 . y
O10 Mo3 O3 153.23(7) . . y
O10 Mo3 O8 85.97(7) . 2_665 y
O10 Mo3 O9 71.94(6) . . y
O4 Cr1 O4 180.0 2_665 . y
O4 Cr1 O8 83.07(7) 2_665 . y
O4 Cr1 O8 83.07(7) . 2_665 y
O4 Cr1 O8 96.93(7) . . y
O4 Cr1 O8 96.93(7) 2_665 2_665 y
O4 Cr1 O9 97.28(7) 2_665 2_665 y
O4 Cr1 O9 82.72(7) 2_665 . y
O4 Cr1 O9 97.28(7) . . y
O4 Cr1 O9 82.72(7) . 2_665 y
O8 Cr1 O8 180.0 . 2_665 y
O9 Cr1 O8 83.66(7) . 2_665 y
O9 Cr1 O8 83.66(7) 2_665 . y
O9 Cr1 O8 96.34(7) . . y
O9 Cr1 O8 96.34(7) 2_665 2_665 y
O9 Cr1 O9 180.0 2_665 . y
Mo3 O3 Mo2 114.24(8) . . ?
Mo1 O4 Mo2 93.92(6) 2_665 . ?
Cr1 O4 Mo1 104.00(7) . 2_665 ?
Cr1 O4 Mo2 101.72(7) . . ?
Mo2 O8 Mo3 95.61(6) 2_665 2_665 ?
Cr1 O8 Mo2 103.83(7) . 2_665 ?
Cr1 O8 Mo3 102.70(7) . 2_665 ?
Mo3 O9 Mo1 94.15(6) . . ?
Cr1 O9 Mo1 103.16(7) . . ?
Cr1 O9 Mo3 101.70(7) . . ?
Mo1 O10 Mo3 117.98(9) . . ?
Mo2 O13 Mo1 117.32(8) 2_665 . ?
C2 N1 C1 122.2(4) . . ?
C6 N2 C5 127.0(3) . . ?
C10 N3 C11 120.9(4) . . ?
N1 C1 C5 119.6(4) . . ?
N3 C11 C7 121.8(4) . . ?
N1 C2 C3 120.1(4) . . ?
C2 C3 C4 118.9(4) . . ?
C5 C4 C3 120.3(4) . . ?
C1 C5 N2 123.2(4) . . ?
C4 C5 N2 118.0(3) . . ?
C4 C5 C1 118.8(4) . . ?
O1 C6 N2 123.2(4) . . ?
O1 C6 C7 119.8(4) . . ?
N2 C6 C7 117.0(3) . . ?
C11 C7 C6 124.1(4) . . ?
C11 C7 C8 117.8(4) . . ?
C8 C7 C6 118.0(4) . . ?
C7 C8 C9 118.4(6) . . ?
C10 C9 C8 119.1(7) . . ?
N3 C10 C9 122.0(6) . . ?
C2A N1A C1A 118(2) . . ?
C6A N2A C5A 128.4(12) . . ?
C9A N3A C8A 120.5(16) . . ?
N1A C1A C5A 120.8(19) . . ?
C3A C2A N1A 122(2) . . ?
C4A C3A C2A 119.3(18) . . ?
C3A C4A C5A 121.7(17) . . ?
C1A C5A N2A 123.6(15) . . ?
C4A C5A N2A 118.5(15) . . ?
C4A C5A C1A 117.9(15) . . ?
O1A C6A N2A 126.6(16) . . ?
O1A C6A C7A 116.2(16) . . ?
N2A C6A C7A 117.1(11) . . ?
C8A C7A C6A 125.5(14) . . ?
C8A C7A C11A 119.4(14) . . ?
C11A C7A C6A 115.1(14) . . ?
C7A C8A N3A 121.7(15) . . ?
N3A C9A C10A 118.0(17) . . ?
C9A C10A C11A 124.4(18) . . ?
C7A C11A C10A 114.6(17) . . ?
_iucr_refine_instructions_details
;
1.res created by SHELXL-2014/7
TITL 1 in P-1
CELL 0.71069 6.021 12.32 13.294 77.871 77.259 79.486
ZERR 1 0.0005 0.0009 0.001 0.001 0.001 0.001
LATT 1
SFAC C H Cr Mo N O
UNIT 22 28 1 6 6 27
EQIV $1 3-X,1-Y,-1-Z
SADI O1 C6 O1A C6A
SADI N1 C1 N1A C1A
SADI N1 C2 N1A C2A
SADI C1 C5 C1A C5A
SADI N2 C5 N2A C5A
SADI N2 C6 N2A C6A
SADI C2 C3 C2A C3A
SADI C3 C4 C3A C4A
SADI N3 C11 N3A C8A
SADI N3 C10 N3A C9A
SADI C4 C5 C4A C5A
SADI C6 C7 C6A C7A
SADI C7 C11 C7A C8A
SADI C7 C8 C7A C11A
SADI C9 C10 C10A C9A
SADI C9 C8 C10A C11A
SADI 0.04 O1 N2 O1A N2A
SADI 0.04 O1 C7 O1A C7A
SADI 0.04 N1 C3 N1A C3A
SADI 0.04 N1 C5 N1A C5A
SADI 0.04 C1 N2 C1A N2A
SADI 0.04 C1 C2 C1A C2A
SADI 0.04 C1 C4 C1A C4A
SADI 0.04 N2 C4 N2A C4A
SADI 0.04 N2 C7 N2A C7A
SADI 0.04 C2 C4 C2A C4A
SADI 0.04 C3 C5 C3A C5A
SADI 0.04 N3 C7 N3A C7A
SADI 0.04 N3 C9 N3A C10A
SADI 0.04 C5 C6 C5A C6A
SADI 0.04 C6 C11 C6A C8A
SADI 0.04 C6 C8 C6A C11A
SADI 0.04 C7 C9 C7A C10A
SADI 0.04 C11 C10 C8A C9A
SADI 0.04 C11 C8 C8A C11A
SADI 0.04 C10 C8 C9A C11A
DELU 0.001 0.001 C6 C7
RIGU 0.001 0.001 O1A > C11A
RIGU O1 > C10
L.S. 12
PLAN 5
FREE H1Wa H1Wb_$1
bump
LIST 1
fmap 2
acta
MERG 2
OMIT -2 2 1
OMIT 1 5 3
OMIT 1 -3 2
OMIT -1 -3 3
OMIT 1 1 6
OMIT 2 0 5
OMIT -1 -3 2
OMIT -3 5 2
OMIT 1 1 5
OMIT 1 0 5
OMIT -1 1 0
OMIT -1 -2 2
OMIT 2 -1 3
OMIT -2 3 4
OMIT 1 -2 1
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.029000 0.183700
FVAR 0.11628
MO1 4 0.563627 0.627513 -0.250097 11.00000 0.02173 0.01841 =
0.01715 -0.00307 -0.00514 -0.00193
MO2 4 0.673784 0.606808 0.172909 11.00000 0.01366 0.02365 =
0.02402 -0.01246 -0.00544 -0.00038
MO3 4 0.728277 0.734710 -0.072825 11.00000 0.01268 0.01516 =
0.02859 -0.00494 -0.00501 -0.00153
CR1 3 0.500000 0.500000 0.000000 10.50000 0.01043 0.01492 =
0.01545 -0.00367 -0.00348 -0.00066
O2 6 0.942298 0.631497 0.177843 11.00000 0.01838 0.03128 =
0.03686 -0.01189 -0.01092 -0.00005
O3 6 0.579489 0.739657 0.072633 11.00000 0.01803 0.02196 =
0.02654 -0.00825 -0.00450 0.00282
O4 6 0.374352 0.537169 0.140456 11.00000 0.01202 0.01944 =
0.01791 -0.00621 -0.00307 -0.00029
AFIX 13
H4B 2 0.221150 0.581405 0.151826 11.00000 -1.20000
AFIX 0
O5 6 1.000165 0.757799 -0.071283 11.00000 0.01682 0.02449 =
0.03577 -0.00810 -0.00581 -0.00294
O6 6 0.494463 0.658258 0.276153 11.00000 0.02703 0.03305 =
0.02741 -0.01416 -0.00249 -0.00121
O7 6 0.591099 0.861705 -0.120049 11.00000 0.02590 0.02246 =
0.03837 -0.00104 -0.00958 0.00002
O8 6 0.226565 0.440215 -0.015829 11.00000 0.01170 0.01990 =
0.02223 -0.00607 -0.00435 -0.00175
PART -1
AFIX 13
H8B 2 0.076188 0.485741 0.000434 10.50000 -1.20000
AFIX 0
PART 0
O9 6 0.427411 0.651401 -0.081026 11.00000 0.01286 0.01544 =
0.02163 -0.00458 -0.00426 0.00069
AFIX 13
H9B 2 0.271767 0.691687 -0.063787 11.00000 -1.20000
AFIX 0
O10 6 0.809484 0.666913 -0.198570 11.00000 0.02476 0.02683 =
0.02487 -0.00903 0.00132 -0.00821
O11 6 0.432247 0.756347 -0.300437 11.00000 0.04946 0.02186 =
0.03026 -0.00118 -0.01428 0.00134
O12 6 0.727395 0.572783 -0.354324 11.00000 0.04862 0.03086 =
0.02356 -0.00752 0.00108 -0.00460
O13 6 0.291690 0.552192 -0.226868 11.00000 0.02866 0.02102 =
0.02954 -0.00469 -0.01675 0.00023
PART 1
O1 6 0.687583 0.992392 -0.398756 10.80000 0.04365 0.04271 =
0.05622 -0.02802 -0.03064 0.01747
N1 5 0.779431 1.128473 -0.157307 10.80000 0.01754 0.01917 =
0.03572 -0.01052 -0.00262 0.00059
AFIX 43
H1 2 0.654847 1.172640 -0.139922 10.80000 -1.20000
AFIX 0
N2 5 1.004002 0.919370 -0.328332 10.80000 0.02593 0.02563 =
0.02790 -0.01219 -0.01012 0.00720
AFIX 43
H2 2 1.122681 0.868514 -0.331992 10.80000 -1.20000
AFIX 0
N3 5 1.132345 0.668801 -0.516389 10.80000 0.03382 0.04916 =
0.05138 -0.03048 -0.00678 0.00604
AFIX 43
H3 2 1.248990 0.617114 -0.512926 10.40000 -1.20000
AFIX 0
C1 1 0.790831 1.067745 -0.232637 10.80000 0.02458 0.02897 =
0.03941 -0.01390 -0.01025 0.00352
AFIX 43
H1A 2 0.668917 1.077155 -0.267588 10.80000 -1.20000
AFIX 0
C11 1 1.093158 0.747394 -0.455822 10.80000 0.03426 0.05047 =
0.04976 -0.03273 -0.01685 0.00947
AFIX 43
H11 2 1.193398 0.744852 -0.410964 10.80000 -1.20000
AFIX 0
C2 1 0.955006 1.122115 -0.109112 10.80000 0.02375 0.02512 =
0.03585 -0.01915 -0.00414 0.00602
AFIX 43
H2A 2 0.943443 1.167159 -0.059617 10.80000 -1.20000
AFIX 0
C3 1 1.153412 1.048869 -0.132617 10.80000 0.03091 0.02939 =
0.03549 -0.01714 -0.01057 0.00297
AFIX 43
H3A 2 1.275945 1.043561 -0.098933 10.80000 -1.20000
AFIX 0
C4 1 1.167424 0.983023 -0.207524 10.80000 0.02369 0.02539 =
0.03133 -0.01304 -0.00687 0.00276
AFIX 43
H4 2 1.300132 0.933114 -0.224066 10.80000 -1.20000
AFIX 0
C5 1 0.985447 0.991427 -0.257345 10.80000 0.02321 0.01585 =
0.02413 -0.00391 -0.00545 0.00012
C6 1 0.855321 0.921079 -0.391850 10.80000 0.02911 0.02693 =
0.02609 -0.00826 -0.00837 -0.00114
C7 1 0.908897 0.831492 -0.458341 10.80000 0.02330 0.02820 =
0.02307 -0.00795 -0.00414 -0.00091
C8 1 0.758773 0.831155 -0.523520 10.80000 0.03676 0.03339 =
0.02872 -0.00350 -0.01317 -0.00576
AFIX 43
H8 2 0.626414 0.883530 -0.524425 10.80000 -1.20000
AFIX 0
C9 1 0.811708 0.749072 -0.588812 10.80000 0.05756 0.05150 =
0.03681 -0.01863 -0.01788 -0.00365
AFIX 43
H9 2 0.720285 0.749839 -0.637016 10.80000 -1.20000
AFIX 0
C10 1 0.996547 0.669808 -0.580071 10.80000 0.04355 0.04539 =
0.03591 -0.01774 -0.00227 -0.00390
AFIX 43
H10 2 1.027607 0.614173 -0.620943 10.80000 -1.20000
AFIX 0
PART 0
PART 2
O1A 6 0.698426 1.011303 -0.393258 10.20000 0.05002 0.03537 =
0.04541 -0.02362 -0.02476 0.01276
N1A 5 0.771911 0.757941 -0.572571 10.20000 0.02989 0.02582 =
0.01586 -0.00644 -0.00135 -0.00336
AFIX 43
H1AC 2 0.651173 0.767645 -0.599772 10.15000 -1.20000
AFIX 0
N2A 5 0.995587 0.866506 -0.381314 10.20000 0.03835 0.02627 =
0.02898 -0.01287 -0.01206 0.00271
AFIX 43
H2AA 2 1.109715 0.842300 -0.349559 10.20000 -1.20000
AFIX 0
N3A 5 1.162673 1.031391 -0.160338 10.20000 0.03377 0.03648 =
0.04152 -0.02478 -0.01264 0.00772
AFIX 43
H3AA 2 1.293193 1.013567 -0.140485 10.15000 -1.20000
AFIX 0
C1A 1 0.798108 0.829242 -0.510653 10.20000 0.04148 0.03371 =
0.03543 -0.01910 -0.01650 0.00667
AFIX 43
H1AB 2 0.696709 0.895580 -0.506848 10.20000 -1.20000
AFIX 0
C2A 1 0.942834 0.671801 -0.589315 10.20000 0.03541 0.03550 =
0.03722 -0.02132 -0.01288 0.00386
AFIX 43
H2AB 2 0.939902 0.629203 -0.638936 10.20000 -1.20000
AFIX 0
C3A 1 1.117471 0.646135 -0.535824 10.20000 0.03986 0.03434 =
0.04359 -0.02396 -0.01762 0.00599
AFIX 43
H3AB 2 1.225314 0.582583 -0.543809 10.20000 -1.20000
AFIX 0
C4A 1 1.133850 0.713514 -0.470800 10.20000 0.04143 0.03294 =
0.04342 -0.02265 -0.01963 0.00768
AFIX 43
H4A 2 1.258393 0.697730 -0.436726 10.20000 -1.20000
AFIX 0
C5A 1 0.973610 0.803604 -0.453812 10.20000 0.03405 0.02285 =
0.02221 -0.00816 -0.00684 -0.00123
C6A 1 0.860955 0.960242 -0.354730 10.20000 0.02923 0.01888 =
0.01957 -0.00418 -0.00141 -0.00535
C7A 1 0.920895 1.009226 -0.270423 10.20000 0.02749 0.01633 =
0.01864 -0.00299 -0.00053 -0.00524
C8A 1 1.118632 0.980012 -0.233228 10.20000 0.03111 0.02459 =
0.02886 -0.01273 -0.00620 0.00053
AFIX 43
H8A 2 1.227627 0.923179 -0.258185 10.20000 -1.20000
AFIX 0
C9A 1 1.008838 1.107464 -0.120228 10.20000 0.02920 0.02511 =
0.03185 -0.01459 -0.00613 0.00077
AFIX 43
H9A 2 1.030396 1.136742 -0.064621 10.20000 -1.20000
AFIX 0
C10A 1 0.821153 1.141832 -0.160889 10.20000 0.02745 0.02350 =
0.02876 -0.01184 -0.00352 -0.00120
AFIX 43
H10A 2 0.727354 1.206244 -0.142581 10.20000 -1.20000
AFIX 0
C11A 1 0.754319 1.087898 -0.229486 10.20000 0.02870 0.02252 =
0.02701 -0.00981 -0.00326 -0.00239
AFIX 43
H11A 2 0.608181 1.104198 -0.245997 10.20000 -1.20000
AFIX 6
PART 0
O1W 6 1.500000 0.500000 -0.500000 10.50000 0.12273 0.08423 =
0.09862 -0.04133 -0.08254 0.04466
H1WA 2 1.434823 0.473285 -0.537975 10.50000 -1.50000
H1WB 2 1.526646 0.450054 -0.447615 10.50000 -1.50000
AFIX 0
HKLF 4
REM 1 in P-1
REM R1 = 0.0230 for 4048 Fo > 4sig(Fo) and 0.0275 for all 4541 data
REM 421 parameters refined using 256 restraints
END
WGHT 0.0290 0.1837
REM Highest difference peak 0.468, deepest hole -0.512, 1-sigma level 0.097
Q1 1 0.5203 0.7021 -0.2859 11.00000 0.05 0.47
Q2 1 0.7590 0.6605 -0.0440 11.00000 0.05 0.41
Q3 1 0.6899 0.8071 -0.1015 11.00000 0.05 0.40
Q4 1 0.7008 0.7124 -0.1646 11.00000 0.05 0.37
Q5 1 0.6622 0.6729 0.1166 11.00000 0.05 0.37
REM The information below was added by Olex2.
REM
REM R1 = 0.0230 for 4048 Fo > 4sig(Fo) and 0.0275 for all 6872 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.47, deepest hole -0.51
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0275
REM R1_gt = 0.0230
REM wR_ref = 0.0559
REM GOOF = 1.036
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 6872
REM Reflections_gt = 4048
REM Parameters = n/a
REM Hole = -0.51
REM Peak = 0.47
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_5
_database_code_depnum_ccdc_archive 'CCDC 1540701'
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT415_5
;
PROBLEM: Short Inter D-H..H-X H1WA .. H16A .. 2.04 Ang.
RESPONSE: This is due to disordered solvate water molecule in the structure.
;
_vrf_PLAT417_5
;
PROBLEM: Short Inter D-H..H-D H2 .. H10B .. 2.07 Ang.
RESPONSE: This is due to disordered solvate water molecule in the structure.
;
# end Validation Reply Form
_audit_creation_date 2017-10-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'Co Cr H14 Mo6 O28, Cr H6 Mo6 O24, C24 H30 Co2 N6 O12, 7(H2 O), 2(C2 H6 O)'
_chemical_formula_sum 'C28 H76 Co3 Cr2 Mo12 N6 O73'
_chemical_formula_weight 3097.01
_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'
Cr Cr 0.3209 0.6236 '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 12.3636(5)
_cell_length_b 13.0466(5)
_cell_length_c 14.4949(5)
_cell_angle_alpha 106.0600(10)
_cell_angle_beta 97.8180(10)
_cell_angle_gamma 111.8130(10)
_cell_volume 2009.83(13)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 8814
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.283
_cell_measurement_theta_min 2.14
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.789
_exptl_absorpt_correction_T_max 0.677
_exptl_absorpt_correction_T_min 0.612
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour pink
_exptl_crystal_colour_primary pink
_exptl_crystal_density_diffrn 2.559
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1503
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.14
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0144
_diffrn_reflns_av_unetI/netI 0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 14801
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.283
_diffrn_reflns_theta_min 1.799
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8622
_reflns_number_total 9866
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_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 'Bruker SHELXTL'
_refine_diff_density_max 0.893
_refine_diff_density_min -1.327
_refine_diff_density_rms 0.113
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 618
_refine_ls_number_reflns 9866
_refine_ls_number_restraints 70
_refine_ls_R_factor_all 0.0343
_refine_ls_R_factor_gt 0.0283
_refine_ls_restrained_S_all 1.071
_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^)+(0.0365P)^2^+2.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0711
_refine_ls_wR_factor_ref 0.0744
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, H23 of O23, H24 of O24, H27 of O27, H9A of O9, H10A of O10,
H12A of O12, {H5WA,H5WB} of O5W, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, {H1WA,H1WB} of O1W, {H2WA,H2WB} of O2W, H30 of O30,
H29 of O29, {H4WA,H4WB} of O4W, {H3WA,H3WB} of O3W, {H8WA,H8WB} of O8W, {H7WA,
H7WB} of O7W, {H6WA,H6WB} of O6W
2. Restrained distances
C16-C15 = C13-C14
1.52 with sigma of 0.02
C16-O29 = O30-C13
1.42 with sigma of 0.02
H10B-O10W
0.85 with sigma of 0.001
O10W-H10C
0.85 with sigma of 0.001
O30-C13 = C16-O29
1.402 with sigma of 0.02
H10C-H10B
1.389 with sigma of 0.02
C13-C14
1.52 with sigma of 0.02
C15-O29 = C14-O30
2.52 with sigma of 0.04
3. Rigid bond restraints
O29, C15, C16, O30, C13, C14
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O29 \\sim C15 \\sim C16 \\sim O30 \\sim C13 \\sim C14: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
Fixed Sof: O6W(0.5) H6WA(0.5) H6WB(0.5) O29(0.5) H29(0.5) C15(0.5) H15A(0.5)
H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5) H16B(0.5) O30(0.5) H30(0.5) C13(0.5)
H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
6.a Riding coordinates:
O5W(H5WA,H5WB)
6.b Free rotating group:
O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB)
6.c Rotating group:
O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
6.d Ternary CH refined with riding coordinates:
O23(H23), O24(H24), O27(H27), O9(H9A), O10(H10A), O12(H12A)
6.e Secondary CH2 refined with riding coordinates:
C16(H16A,H16B), C13(H13A,H13B)
6.f Aromatic/amide H refined with riding coordinates:
N2(H2), N3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
6.g Tetrahedral OH refined with riding coordinates:
O29(H29), O30(H30)
6.h Idealised Me refined as rotating group:
C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 1.17247(2) 0.59117(2) 0.85218(2) 0.01947(6) Uani 1 1 d . . . . .
Mo2 Mo 1.20590(2) 0.40006(2) 0.95075(2) 0.02108(6) Uani 1 1 d . . . . .
Mo3 Mo 0.96054(3) 0.68428(2) 0.89512(2) 0.02348(7) Uani 1 1 d . . . . .
Co1 Co 1.0000 1.0000 1.0000 0.03057(15) Uani 1 2 d S T P . .
Cr1 Cr 1.0000 0.5000 1.0000 0.01332(12) Uani 1 2 d S T P . .
O1W O 1.1728(3) 1.0592(3) 1.0891(3) 0.0640(10) Uani 1 1 d . . . . .
H1WA H 1.1910 1.0227 1.1343 0.096 Uiso 1 1 d GR . . . .
H1WB H 1.2176 1.1363 1.1388 0.096 Uiso 1 1 d GR . . . .
O2W O 1.0727(3) 1.0241(3) 0.8848(2) 0.0436(7) Uani 1 1 d . . . . .
H2WA H 1.1289 0.9957 0.8779 0.065 Uiso 1 1 d GR . . . .
H2WB H 1.1168 1.1012 0.8958 0.065 Uiso 1 1 d GR . . . .
O17 O 1.1786(3) 0.2557(2) 0.89457(19) 0.0359(6) Uani 1 1 d . . . . .
O18 O 1.1937(2) 0.4023(2) 1.08501(17) 0.0259(5) Uani 1 1 d . . . . .
O19 O 1.1570(2) 0.43430(19) 0.83637(16) 0.0225(4) Uani 1 1 d . . . . .
O20 O 1.3588(2) 0.4770(3) 0.9834(2) 0.0380(6) Uani 1 1 d . . . . .
O21 O 1.1295(2) 0.5721(2) 0.72854(17) 0.0297(5) Uani 1 1 d . . . . .
O22 O 1.3246(2) 0.6715(2) 0.88955(19) 0.0347(6) Uani 1 1 d . . . . .
O23 O 0.97692(18) 0.51236(18) 0.86701(15) 0.0173(4) Uani 1 1 d . . . . .
H23 H 0.9162 0.4430 0.8114 0.021 Uiso 1 1 calc R . . . .
O24 O 1.17355(18) 0.56676(18) 1.00433(15) 0.0182(4) Uani 1 1 d . . . . .
H24 H 1.2308 0.6323 1.0644 0.022 Uiso 1 1 calc R . . . .
O25 O 1.1287(2) 0.71631(19) 0.91205(17) 0.0259(5) Uani 1 1 d . . . . .
O26 O 0.9151(3) 0.6572(3) 0.7721(2) 0.0458(7) Uani 1 1 d . . . . .
O27 O 0.99271(19) 0.65339(18) 1.04482(15) 0.0196(4) Uani 1 1 d . . . . .
H27 H 1.0564 0.7177 1.1022 0.024 Uiso 1 1 calc R . . . .
O28 O 0.9827(3) 0.8268(2) 0.9553(2) 0.0415(7) Uani 1 1 d . . . . .
Mo4 Mo 0.39486(3) -0.28426(2) 0.46838(3) 0.02926(7) Uani 1 1 d . . . . .
Mo5 Mo 0.66635(3) 0.20514(2) 0.72335(2) 0.03114(8) Uani 1 1 d . . . . .
Mo6 Mo 0.54612(3) -0.08238(3) 0.69494(3) 0.03074(7) Uani 1 1 d . . . . .
Cr2 Cr 0.5000 0.0000 0.5000 0.02226(15) Uani 1 2 d S T P . .
O4 O 0.4796(2) -0.3586(2) 0.4861(2) 0.0419(7) Uani 1 1 d . . . . .
O5 O 0.2483(2) -0.3876(2) 0.4336(2) 0.0412(7) Uani 1 1 d . . . . .
O6 O 0.3946(2) -0.2068(2) 0.6046(2) 0.0329(6) Uani 1 1 d . . . . .
O8 O 0.4972(3) -0.0522(3) 0.7989(2) 0.0486(7) Uani 1 1 d . . . . .
O9 O 0.34375(19) -0.14034(18) 0.44214(18) 0.0249(5) Uani 1 1 d . . . . .
H9A H 0.2726 -0.1345 0.4613 0.030 Uiso 1 1 calc R . . . .
O10 O 0.55984(19) -0.10822(19) 0.53445(18) 0.0259(5) Uani 1 1 d . . . . .
H10A H 0.6360 -0.1053 0.5203 0.031 Uiso 1 1 calc R . . . .
O11 O 0.6284(3) -0.1583(2) 0.7125(2) 0.0446(7) Uani 1 1 d . . . . .
O12 O 0.4846(2) 0.04114(19) 0.63856(18) 0.0273(5) Uani 1 1 d . . . . .
H12A H 0.4098 0.0453 0.6500 0.033 Uiso 1 1 calc R . . . .
O13 O 0.6852(2) 0.0676(2) 0.7242(2) 0.0341(6) Uani 1 1 d . . . . .
O14 O 0.6310(3) 0.2457(3) 0.8341(2) 0.0425(7) Uani 1 1 d . . . . .
O15 O 0.5838(2) 0.2758(2) 0.6580(2) 0.0337(6) Uani 1 1 d . . . . .
O16 O 0.8157(2) 0.2988(2) 0.7478(2) 0.0432(7) Uani 1 1 d . . . . .
Co2 Co 0.97488(4) 0.24353(4) 0.46954(3) 0.02003(9) Uani 1 1 d . . . . .
O1 O 0.8665(2) -0.2797(2) 0.41501(17) 0.0267(5) Uani 1 1 d . . . . .
O2 O 0.7507(2) -0.0838(2) 0.46434(19) 0.0291(5) Uani 1 1 d . . . . .
O3 O 0.83182(19) 0.10856(19) 0.48563(17) 0.0237(5) Uani 1 1 d . . . . .
O3W O 0.9590(2) 0.3671(3) 0.5794(2) 0.0451(7) Uani 1 1 d . . . . .
H3WA H 0.8988 0.3840 0.5581 0.068 Uiso 1 1 d GR . . . .
H3WB H 1.0231 0.4366 0.5989 0.068 Uiso 1 1 d GR . . . .
O4W O 1.0973(2) 0.3560(2) 0.4233(2) 0.0341(6) Uani 1 1 d . . . . .
H4WA H 1.0745 0.3363 0.3584 0.051 Uiso 1 1 d GR . . . .
H4WB H 1.1653 0.3488 0.4326 0.051 Uiso 1 1 d GR . . . .
O5W O 0.8317(2) 0.2489(2) 0.36208(18) 0.0300(5) Uani 1 1 d . . . . .
H5WA H 0.7568 0.2207 0.3594 0.036 Uiso 1 1 d R . . . .
H5WB H 0.8825 0.3037 0.3689 0.036 Uiso 1 1 d R . . . .
N1 N 0.9912(2) 0.0890(2) 0.38874(19) 0.0202(5) Uani 1 1 d . . . . .
N2 N 0.7225(2) -0.2843(2) 0.29591(19) 0.0203(5) Uani 1 1 d . . . . .
H2 H 0.7085 -0.2452 0.2605 0.024 Uiso 1 1 calc R . . . .
N3 N 0.4216(2) -0.5219(3) 0.2056(2) 0.0298(6) Uani 1 1 d . . . . .
H3 H 0.3522 -0.5359 0.1707 0.036 Uiso 1 1 calc R . . . .
C1 C 0.8232(3) 0.0036(3) 0.4524(2) 0.0190(6) Uani 1 1 d . . . . .
C2 C 0.9126(2) -0.0116(3) 0.3950(2) 0.0177(5) Uani 1 1 d . . . . .
C3 C 0.9184(3) -0.1185(3) 0.3565(2) 0.0189(6) Uani 1 1 d . . . . .
C4 C 1.0123(3) -0.1206(3) 0.3125(2) 0.0234(6) Uani 1 1 d . . . . .
H4 H 1.0204 -0.1904 0.2879 0.028 Uiso 1 1 calc R . . . .
C5 C 1.0918(3) -0.0176(3) 0.3065(2) 0.0270(7) Uani 1 1 d . . . . .
H5 H 1.1542 -0.0171 0.2770 0.032 Uiso 1 1 calc R . . . .
C6 C 1.0785(3) 0.0855(3) 0.3447(3) 0.0264(7) Uani 1 1 d . . . . .
H6 H 1.1322 0.1545 0.3394 0.032 Uiso 1 1 calc R . . . .
C7 C 0.8326(3) -0.2336(3) 0.3603(2) 0.0201(6) Uani 1 1 d . . . . .
C8 C 0.6282(3) -0.3937(3) 0.2801(2) 0.0197(6) Uani 1 1 d . . . . .
C9 C 0.6411(3) -0.4790(3) 0.3142(3) 0.0320(8) Uani 1 1 d . . . . .
H9 H 0.7160 -0.4651 0.3512 0.038 Uiso 1 1 calc R . . . .
C10 C 0.5416(4) -0.5848(4) 0.2926(3) 0.0449(10) Uani 1 1 d . . . . .
H10 H 0.5498 -0.6428 0.3145 0.054 Uiso 1 1 calc R . . . .
C11 C 0.4309(3) -0.6045(3) 0.2391(3) 0.0404(9) Uani 1 1 d . . . . .
H11 H 0.3632 -0.6745 0.2263 0.049 Uiso 1 1 calc R . . . .
C12 C 0.5150(3) -0.4183(3) 0.2236(2) 0.0248(6) Uani 1 1 d . . . . .
H12 H 0.5044 -0.3632 0.1987 0.030 Uiso 1 1 calc R . . . .
O6W O 1.1839(7) 0.8592(7) 1.1046(6) 0.068(2) Uani 0.5 1 d . . . . .
H6WA H 1.2262 0.8373 1.0691 0.103 Uiso 0.5 1 d G . . . .
H6WB H 1.2274 0.8863 1.1641 0.103 Uiso 0.5 1 d G . . . .
O7W O 1.3220(3) 0.3920(3) 0.4344(3) 0.0609(10) Uani 1 1 d . . . . .
H7WA H 1.3672 0.4654 0.4642 0.091 Uiso 1 1 d G . . . .
H7WB H 1.3634 0.3581 0.4527 0.091 Uiso 1 1 d G . . . .
O8W O 1.2261(3) 0.9365(3) 0.8256(3) 0.0626(9) Uani 1 1 d . . . . .
H8WA H 1.1722 0.8716 0.7829 0.094 Uiso 1 1 d G . . . .
H8WB H 1.2918 0.9298 0.8262 0.094 Uiso 1 1 d G . . . .
O10W O 0.3532(3) 0.1231(3) 0.7696(3) 0.0534(8) Uani 1 1 d D . . . .
H10B H 0.2955(12) 0.1171(18) 0.7968(13) 0.27(7) Uiso 1 1 d D . . . .
H10C H 0.385(2) 0.0836(16) 0.7910(11) 0.42(12) Uiso 1 1 d D . . . .
O29 O 0.3947(11) -0.0859(10) 1.0004(9) 0.134(4) Uani 0.5 1 d D U . A 1
H29 H 0.3796 -0.1458 1.0142 0.201 Uiso 0.5 1 calc R . . A 1
C15 C 0.3725(11) 0.0755(11) 1.0182(10) 0.113(4) Uani 0.5 1 d D U . A 1
H15A H 0.4569 0.1086 1.0514 0.169 Uiso 0.5 1 calc GR . . A 1
H15B H 0.3353 0.1190 1.0558 0.169 Uiso 0.5 1 calc GR . . A 1
H15C H 0.3633 0.0800 0.9528 0.169 Uiso 0.5 1 calc GR . . A 1
C16 C 0.3120(10) -0.0536(9) 1.0096(7) 0.066(3) Uani 0.5 1 d D U . A 1
H16A H 0.2866 -0.0606 1.0689 0.079 Uiso 0.5 1 calc R . . A 1
H16B H 0.2426 -0.0994 0.9518 0.079 Uiso 0.5 1 calc R . . A 1
O30 O 0.4526(5) 0.2856(6) 0.9651(5) 0.0527(16) Uani 0.5 1 d D U . B 2
H30 H 0.4499 0.2384 0.9129 0.079 Uiso 0.5 1 calc R . . B 2
C13 C 0.3912(13) 0.2278(12) 1.0159(9) 0.113(4) Uani 0.5 1 d D U . B 2
H13A H 0.3123 0.1805 0.9685 0.135 Uiso 0.5 1 calc R . . B 2
H13B H 0.3812 0.2896 1.0642 0.135 Uiso 0.5 1 calc R . . B 2
C14 C 0.3965(13) 0.1524(12) 1.0710(11) 0.126(4) Uani 0.5 1 d D U . B 2
H14A H 0.3257 0.0785 1.0423 0.189 Uiso 0.5 1 calc GR . . B 2
H14B H 0.4002 0.1900 1.1392 0.189 Uiso 0.5 1 calc GR . . B 2
H14C H 0.4672 0.1386 1.0683 0.189 Uiso 0.5 1 calc GR . . B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.02184(13) 0.01923(12) 0.01852(13) 0.00749(10) 0.00796(10) 0.00861(10)
Mo2 0.02239(13) 0.02533(14) 0.02232(13) 0.01014(11) 0.00795(10) 0.01549(11)
Mo3 0.03433(15) 0.02511(14) 0.02485(14) 0.01575(11) 0.01365(11) 0.02034(12)
Co1 0.0456(4) 0.0245(3) 0.0337(4) 0.0143(3) 0.0149(3) 0.0233(3)
Cr1 0.0149(3) 0.0138(3) 0.0123(3) 0.0049(2) 0.0028(2) 0.0074(2)
O1W 0.066(2) 0.074(2) 0.0466(19) 0.0100(17) -0.0024(16) 0.040(2)
O2W 0.0662(19) 0.0374(15) 0.0462(16) 0.0232(13) 0.0259(14) 0.0324(15)
O17 0.0534(16) 0.0357(14) 0.0355(14) 0.0167(12) 0.0216(12) 0.0307(13)
O18 0.0275(11) 0.0356(13) 0.0247(12) 0.0144(10) 0.0086(9) 0.0207(10)
O19 0.0291(11) 0.0221(11) 0.0197(11) 0.0068(9) 0.0094(9) 0.0139(9)
O20 0.0253(12) 0.0547(17) 0.0415(15) 0.0220(13) 0.0117(11) 0.0204(12)
O21 0.0391(13) 0.0280(12) 0.0242(12) 0.0125(10) 0.0109(10) 0.0137(11)
O22 0.0259(12) 0.0339(14) 0.0382(15) 0.0104(11) 0.0106(11) 0.0075(11)
O23 0.0188(10) 0.0174(10) 0.0143(9) 0.0052(8) 0.0022(8) 0.0073(8)
O24 0.0163(9) 0.0187(10) 0.0161(10) 0.0038(8) 0.0022(8) 0.0064(8)
O25 0.0315(12) 0.0166(10) 0.0316(12) 0.0097(9) 0.0148(10) 0.0096(9)
O26 0.0591(18) 0.071(2) 0.0329(15) 0.0340(15) 0.0183(13) 0.0413(17)
O27 0.0212(10) 0.0158(10) 0.0212(11) 0.0049(8) 0.0048(8) 0.0088(8)
O28 0.0596(18) 0.0286(13) 0.0600(18) 0.0257(13) 0.0344(15) 0.0303(13)
Mo4 0.02206(14) 0.01389(12) 0.04972(19) 0.00699(12) 0.01555(13) 0.00661(11)
Mo5 0.02447(14) 0.01728(13) 0.03882(18) -0.00321(12) 0.01383(12) 0.00322(11)
Mo6 0.02608(14) 0.02315(14) 0.04363(18) 0.01187(13) 0.01627(13) 0.00885(12)
Cr2 0.0175(3) 0.0116(3) 0.0349(4) 0.0034(3) 0.0132(3) 0.0048(3)
O4 0.0321(14) 0.0273(13) 0.070(2) 0.0146(13) 0.0183(13) 0.0172(11)
O5 0.0271(13) 0.0227(12) 0.068(2) 0.0116(12) 0.0167(13) 0.0064(10)
O6 0.0255(12) 0.0224(12) 0.0506(16) 0.0140(11) 0.0201(11) 0.0060(10)
O8 0.0458(17) 0.0532(19) 0.0487(18) 0.0182(15) 0.0248(14) 0.0190(15)
O9 0.0180(10) 0.0143(10) 0.0385(13) 0.0031(9) 0.0144(9) 0.0052(8)
O10 0.0197(10) 0.0157(10) 0.0422(14) 0.0073(10) 0.0167(10) 0.0067(9)
O11 0.0363(15) 0.0309(14) 0.067(2) 0.0205(14) 0.0136(13) 0.0129(12)
O12 0.0202(11) 0.0192(11) 0.0407(14) 0.0047(10) 0.0174(10) 0.0076(9)
O13 0.0247(12) 0.0229(12) 0.0484(16) 0.0054(11) 0.0144(11) 0.0071(10)
O14 0.0418(15) 0.0391(15) 0.0413(16) 0.0022(12) 0.0193(13) 0.0178(13)
O15 0.0295(12) 0.0183(11) 0.0467(15) -0.0004(10) 0.0173(11) 0.0095(10)
O16 0.0280(13) 0.0238(13) 0.0560(18) -0.0029(12) 0.0120(12) 0.0003(11)
Co2 0.01957(19) 0.0195(2) 0.0222(2) 0.00873(16) 0.00724(16) 0.00808(16)
O1 0.0238(11) 0.0265(12) 0.0270(12) 0.0122(10) -0.0020(9) 0.0089(9)
O2 0.0280(12) 0.0229(11) 0.0384(14) 0.0107(10) 0.0203(10) 0.0093(10)
O3 0.0238(11) 0.0204(11) 0.0312(12) 0.0094(9) 0.0148(9) 0.0113(9)
O3W 0.0266(13) 0.0425(16) 0.0462(17) -0.0109(13) 0.0023(12) 0.0158(12)
O4W 0.0267(12) 0.0421(15) 0.0385(14) 0.0276(12) 0.0104(11) 0.0099(11)
O5W 0.0204(11) 0.0331(13) 0.0374(14) 0.0175(11) 0.0071(10) 0.0091(10)
N1 0.0179(11) 0.0205(12) 0.0208(13) 0.0080(10) 0.0048(10) 0.0066(10)
N2 0.0211(12) 0.0181(12) 0.0212(13) 0.0078(10) 0.0020(10) 0.0085(10)
N3 0.0201(13) 0.0314(15) 0.0308(16) 0.0085(12) -0.0003(11) 0.0079(12)
C1 0.0173(13) 0.0218(14) 0.0181(14) 0.0072(11) 0.0051(11) 0.0084(11)
C2 0.0147(12) 0.0218(14) 0.0157(13) 0.0064(11) 0.0034(10) 0.0073(11)
C3 0.0180(13) 0.0238(15) 0.0144(13) 0.0064(11) 0.0027(11) 0.0091(12)
C4 0.0240(15) 0.0263(16) 0.0220(15) 0.0065(12) 0.0073(12) 0.0142(13)
C5 0.0207(15) 0.0363(18) 0.0276(17) 0.0106(14) 0.0114(13) 0.0147(14)
C6 0.0213(15) 0.0291(17) 0.0296(17) 0.0116(14) 0.0124(13) 0.0089(13)
C7 0.0220(14) 0.0210(14) 0.0171(14) 0.0045(11) 0.0055(11) 0.0104(12)
C8 0.0205(14) 0.0192(14) 0.0182(14) 0.0054(11) 0.0044(11) 0.0084(12)
C9 0.0252(16) 0.0280(18) 0.040(2) 0.0149(15) 0.0003(14) 0.0094(14)
C10 0.037(2) 0.031(2) 0.064(3) 0.028(2) 0.0007(19) 0.0077(17)
C11 0.0290(18) 0.0303(19) 0.051(2) 0.0180(18) 0.0009(17) 0.0019(15)
C12 0.0241(15) 0.0257(16) 0.0248(16) 0.0095(13) 0.0026(12) 0.0118(13)
O6W 0.067(5) 0.061(5) 0.059(5) 0.007(4) -0.004(4) 0.027(4)
O7W 0.0347(16) 0.0488(19) 0.108(3) 0.038(2) 0.0184(17) 0.0195(15)
O8W 0.066(2) 0.049(2) 0.084(3) 0.0214(18) 0.042(2) 0.0307(18)
O10W 0.0449(17) 0.069(2) 0.073(2) 0.0461(19) 0.0233(16) 0.0346(17)
O29 0.130(8) 0.100(7) 0.105(7) -0.005(6) 0.002(6) 0.019(6)
C15 0.092(6) 0.102(6) 0.083(6) 0.013(5) -0.001(5) 0.001(6)
C16 0.067(6) 0.061(5) 0.042(5) 0.010(4) -0.004(4) 0.011(4)
O30 0.026(3) 0.052(4) 0.066(4) 0.003(3) 0.000(3) 0.018(3)
C13 0.087(6) 0.100(6) 0.095(6) 0.003(5) -0.006(5) 0.014(6)
C14 0.104(7) 0.110(8) 0.096(8) 0.017(5) 0.002(6) -0.002(7)
_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
Mo1 O19 1.927(2) . y
Mo1 O21 1.718(2) . y
Mo1 O22 1.695(2) . y
Mo1 O23 2.316(2) . y
Mo1 O24 2.313(2) . y
Mo1 O25 1.927(2) . y
Mo2 O17 1.711(3) . y
Mo2 O18 1.965(2) . y
Mo2 O19 1.911(2) . y
Mo2 O20 1.699(3) . y
Mo2 O24 2.300(2) . y
Mo2 O27 2.305(2) 2_767 y
Mo3 O18 1.930(2) 2_767 y
Mo3 O23 2.257(2) . y
Mo3 O25 1.928(2) . y
Mo3 O26 1.689(3) . y
Mo3 O27 2.323(2) . y
Mo3 O28 1.718(3) . y
Co1 O1W 2.074(3) . y
Co1 O1W 2.074(3) 2_777 y
Co1 O2W 2.045(3) 2_777 y
Co1 O2W 2.045(3) . y
Co1 O28 2.089(2) 2_777 y
Co1 O28 2.089(2) . y
Cr1 O23 1.9697(19) 2_767 y
Cr1 O23 1.9697(19) . y
Cr1 O24 1.978(2) 2_767 y
Cr1 O24 1.978(2) . y
Cr1 O27 1.966(2) 2_767 y
Cr1 O27 1.966(2) . y
O1W H1WA 0.9578 . ?
O1W H1WB 0.9556 . ?
O2W H2WA 0.9055 . ?
O2W H2WB 0.9024 . ?
O18 Mo3 1.930(2) 2_767 y
O23 H23 0.9800 . ?
O24 H24 0.9800 . ?
O27 Mo2 2.305(2) 2_767 y
O27 H27 0.9800 . ?
Mo4 O4 1.710(3) . y
Mo4 O5 1.707(2) . y
Mo4 O6 1.955(3) . y
Mo4 O9 2.298(2) . y
Mo4 O10 2.263(2) . y
Mo4 O15 1.913(3) 2_656 y
Mo5 O9 2.281(2) 2_656 y
Mo5 O12 2.315(2) . y
Mo5 O13 1.896(3) . y
Mo5 O14 1.715(3) . y
Mo5 O15 1.925(3) . y
Mo5 O16 1.713(3) . y
Mo6 O6 1.938(3) . y
Mo6 O8 1.700(3) . y
Mo6 O10 2.296(2) . y
Mo6 O11 1.702(3) . y
Mo6 O12 2.305(3) . y
Mo6 O13 1.951(2) . y
Cr2 O9 1.967(2) 2_656 y
Cr2 O9 1.967(2) . y
Cr2 O10 1.964(2) . y
Cr2 O10 1.964(2) 2_656 y
Cr2 O12 1.985(2) 2_656 y
Cr2 O12 1.985(2) . y
O9 Mo5 2.281(2) 2_656 y
O9 H9A 0.9800 . ?
O10 H10A 0.9800 . ?
O12 H12A 0.9800 . ?
O15 Mo4 1.913(3) 2_656 y
Co2 O1 2.202(2) 2_756 y
Co2 O3 2.076(2) . y
Co2 O3W 2.018(3) . y
Co2 O4W 2.016(2) . y
Co2 O5W 2.228(2) . y
Co2 N1 2.130(3) . y
O1 Co2 2.202(2) 2_756 y
O1 C7 1.236(4) . ?
O2 C1 1.235(4) . ?
O3 C1 1.277(4) . ?
O3W H3WA 0.8925 . ?
O3W H3WB 0.8909 . ?
O4W H4WA 0.8776 . ?
O4W H4WB 0.8763 . ?
O5W H5WA 0.8506 . ?
O5W H5WB 0.7258 . ?
N1 C2 1.348(4) . ?
N1 C6 1.336(4) . ?
N2 H2 0.8600 . ?
N2 C7 1.344(4) . ?
N2 C8 1.400(4) . ?
N3 H3 0.8600 . ?
N3 C11 1.332(5) . ?
N3 C12 1.338(4) . ?
C1 C2 1.509(4) . ?
C2 C3 1.383(4) . ?
C3 C4 1.403(4) . ?
C3 C7 1.503(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(5) . ?
C6 H6 0.9300 . ?
C8 C9 1.387(5) . ?
C8 C12 1.393(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.382(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.372(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O6W H6WA 0.8504 . ?
O6W H6WB 0.8504 . ?
O7W H7WA 0.8499 . ?
O7W H7WB 0.8502 . ?
O8W H8WA 0.8499 . ?
O8W H8WB 0.8483 . ?
O10W H10B 0.8501(10) . ?
O10W H10C 0.8501(10) . ?
O29 H29 0.8200 . ?
O29 C16 1.252(11) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C16 1.528(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O30 H30 0.8200 . ?
O30 C13 1.311(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.442(12) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Mo1 O23 82.37(8) . . y
O19 Mo1 O24 71.46(8) . . y
O21 Mo1 O19 98.57(10) . . y
O21 Mo1 O23 94.92(10) . . y
O21 Mo1 O24 162.30(10) . . y
O21 Mo1 O25 100.48(11) . . y
O22 Mo1 O19 102.01(11) . . y
O22 Mo1 O21 105.84(12) . . y
O22 Mo1 O23 157.73(10) . . y
O22 Mo1 O24 90.79(10) . . y
O22 Mo1 O25 97.82(12) . . y
O24 Mo1 O23 69.69(7) . . y
O25 Mo1 O19 147.49(9) . . y
O25 Mo1 O23 69.99(8) . . y
O25 Mo1 O24 82.84(9) . . y
O17 Mo2 O18 100.23(11) . . y
O17 Mo2 O19 99.86(11) . . y
O17 Mo2 O24 160.70(11) . . y
O17 Mo2 O27 91.57(11) . 2_767 y
O18 Mo2 O24 81.03(9) . . y
O18 Mo2 O27 70.83(8) . 2_767 y
O19 Mo2 O18 148.21(9) . . y
O19 Mo2 O24 72.03(8) . . y
O19 Mo2 O27 84.24(8) . 2_767 y
O20 Mo2 O17 105.17(14) . . y
O20 Mo2 O18 95.75(11) . . y
O20 Mo2 O19 102.44(11) . . y
O20 Mo2 O24 93.80(11) . . y
O20 Mo2 O27 160.39(11) . 2_767 y
O24 Mo2 O27 70.50(7) . 2_767 y
O18 Mo3 O23 83.91(9) 2_767 . y
O18 Mo3 O27 71.00(8) 2_767 . y
O23 Mo3 O27 70.79(7) . . y
O25 Mo3 O18 148.51(9) . 2_767 y
O25 Mo3 O23 71.32(8) . . y
O25 Mo3 O27 82.43(9) . . y
O26 Mo3 O18 98.81(13) . 2_767 y
O26 Mo3 O23 92.49(12) . . y
O26 Mo3 O25 101.33(12) . . y
O26 Mo3 O27 160.90(13) . . y
O26 Mo3 O28 106.13(15) . . y
O28 Mo3 O18 100.39(12) . 2_767 y
O28 Mo3 O23 159.85(12) . . y
O28 Mo3 O25 96.96(12) . . y
O28 Mo3 O27 91.84(11) . . y
O1W Co1 O1W 180.00(19) 2_777 . y
O1W Co1 O28 89.83(14) 2_777 . y
O1W Co1 O28 90.17(14) . . y
O1W Co1 O28 90.17(14) 2_777 2_777 y
O1W Co1 O28 89.83(14) . 2_777 y
O2W Co1 O1W 89.04(14) . . y
O2W Co1 O1W 89.04(14) 2_777 2_777 y
O2W Co1 O1W 90.96(14) 2_777 . y
O2W Co1 O1W 90.96(14) . 2_777 y
O2W Co1 O2W 180.00(17) . 2_777 y
O2W Co1 O28 90.01(11) . 2_777 y
O2W Co1 O28 89.99(11) 2_777 2_777 y
O2W Co1 O28 89.99(11) . . y
O2W Co1 O28 90.01(11) 2_777 . y
O28 Co1 O28 180.0 . 2_777 y
O23 Cr1 O23 180.00(13) 2_767 . y
O23 Cr1 O24 84.14(8) . . y
O23 Cr1 O24 84.14(8) 2_767 2_767 y
O23 Cr1 O24 95.86(8) . 2_767 y
O23 Cr1 O24 95.86(8) 2_767 . y
O24 Cr1 O24 180.0 . 2_767 y
O27 Cr1 O23 95.23(9) . 2_767 y
O27 Cr1 O23 84.77(9) 2_767 2_767 y
O27 Cr1 O23 84.76(9) . . y
O27 Cr1 O23 95.23(9) 2_767 . y
O27 Cr1 O24 95.26(9) . . y
O27 Cr1 O24 84.74(9) . 2_767 y
O27 Cr1 O24 84.74(9) 2_767 . y
O27 Cr1 O24 95.26(9) 2_767 2_767 y
O27 Cr1 O27 180.0 . 2_767 y
Co1 O1W H1WA 122.6 . . ?
Co1 O1W H1WB 124.1 . . ?
H1WA O1W H1WB 91.8 . . ?
Co1 O2W H2WA 113.0 . . ?
Co1 O2W H2WB 112.1 . . ?
H2WA O2W H2WB 101.3 . . ?
Mo3 O18 Mo2 119.86(12) 2_767 . ?
Mo2 O19 Mo1 119.59(11) . . ?
Mo1 O23 H23 117.7 . . ?
Mo3 O23 Mo1 93.63(7) . . ?
Mo3 O23 H23 117.7 . . ?
Cr1 O23 Mo1 103.15(8) . . ?
Cr1 O23 Mo3 103.33(9) . . ?
Cr1 O23 H23 117.7 . . ?
Mo1 O24 H24 118.4 . . ?
Mo2 O24 Mo1 91.97(7) . . ?
Mo2 O24 H24 118.4 . . ?
Cr1 O24 Mo1 103.02(8) . . ?
Cr1 O24 Mo2 102.29(9) . . ?
Cr1 O24 H24 118.4 . . ?
Mo1 O25 Mo3 119.80(11) . . ?
Mo2 O27 Mo3 93.49(8) 2_767 . ?
Mo2 O27 H27 118.5 2_767 . ?
Mo3 O27 H27 118.5 . . ?
Cr1 O27 Mo2 102.46(9) . 2_767 ?
Cr1 O27 Mo3 101.10(9) . . ?
Cr1 O27 H27 118.5 . . ?
Mo3 O28 Co1 168.64(18) . . ?
O4 Mo4 O6 101.96(13) . . y
O4 Mo4 O9 160.26(10) . . y
O4 Mo4 O10 91.73(11) . . y
O4 Mo4 O15 98.75(13) . 2_656 y
O5 Mo4 O4 104.94(13) . . y
O5 Mo4 O6 95.34(12) . . y
O5 Mo4 O9 93.87(11) . . y
O5 Mo4 O10 161.01(11) . . y
O5 Mo4 O15 100.53(13) . 2_656 y
O6 Mo4 O9 81.85(10) . . y
O6 Mo4 O10 71.93(9) . . y
O10 Mo4 O9 70.83(8) . . y
O15 Mo4 O6 149.62(10) 2_656 . y
O15 Mo4 O9 71.44(9) 2_656 . y
O15 Mo4 O10 85.54(9) 2_656 . y
O9 Mo5 O12 70.39(8) 2_656 . y
O13 Mo5 O9 85.54(10) . 2_656 y
O13 Mo5 O12 71.01(10) . . y
O13 Mo5 O15 148.26(11) . . y
O14 Mo5 O9 163.22(12) . 2_656 y
O14 Mo5 O12 96.97(11) . . y
O14 Mo5 O13 101.08(13) . . y
O14 Mo5 O15 95.90(13) . . y
O15 Mo5 O9 71.64(9) . 2_656 y
O15 Mo5 O12 80.51(10) . . y
O16 Mo5 O9 89.64(11) . 2_656 y
O16 Mo5 O12 157.71(11) . . y
O16 Mo5 O13 98.41(12) . . y
O16 Mo5 O14 104.43(14) . . y
O16 Mo5 O15 103.08(13) . . y
O6 Mo6 O10 71.47(9) . . y
O6 Mo6 O12 84.69(10) . . y
O6 Mo6 O13 148.97(12) . . y
O8 Mo6 O6 98.30(13) . . y
O8 Mo6 O10 160.33(13) . . y
O8 Mo6 O11 105.94(16) . . y
O8 Mo6 O12 92.31(13) . . y
O8 Mo6 O13 100.78(13) . . y
O10 Mo6 O12 70.44(8) . . y
O11 Mo6 O6 102.34(13) . . y
O11 Mo6 O10 92.86(12) . . y
O11 Mo6 O12 159.05(12) . . y
O11 Mo6 O13 95.67(12) . . y
O13 Mo6 O10 82.69(10) . . y
O13 Mo6 O12 70.36(10) . . y
O9 Cr2 O9 180.0 2_656 . y
O9 Cr2 O12 84.17(9) 2_656 . y
O9 Cr2 O12 84.17(9) . 2_656 y
O9 Cr2 O12 95.83(9) . . y
O9 Cr2 O12 95.83(9) 2_656 2_656 y
O10 Cr2 O9 95.46(9) . 2_656 y
O10 Cr2 O9 84.54(9) 2_656 2_656 y
O10 Cr2 O9 95.47(9) 2_656 . y
O10 Cr2 O9 84.54(9) . . y
O10 Cr2 O10 180.0 . 2_656 y
O10 Cr2 O12 95.57(10) 2_656 . y
O10 Cr2 O12 84.43(10) 2_656 2_656 y
O10 Cr2 O12 95.57(10) . 2_656 y
O10 Cr2 O12 84.43(10) . . y
O12 Cr2 O12 180.0 2_656 . y
Mo6 O6 Mo4 117.75(11) . . ?
Mo4 O9 H9A 118.3 . . ?
Mo5 O9 Mo4 92.59(8) 2_656 . ?
Mo5 O9 H9A 118.3 2_656 . ?
Cr2 O9 Mo4 101.60(10) . . ?
Cr2 O9 Mo5 103.58(9) . 2_656 ?
Cr2 O9 H9A 118.3 . . ?
Mo4 O10 Mo6 93.91(8) . . ?
Mo4 O10 H10A 117.8 . . ?
Mo6 O10 H10A 117.8 . . ?
Cr2 O10 Mo4 102.94(10) . . ?
Cr2 O10 Mo6 103.05(9) . . ?
Cr2 O10 H10A 117.8 . . ?
Mo5 O12 H12A 118.5 . . ?
Mo6 O12 Mo5 93.31(9) . . ?
Mo6 O12 H12A 118.5 . . ?
Cr2 O12 Mo5 101.80(9) . . ?
Cr2 O12 Mo6 102.04(9) . . ?
Cr2 O12 H12A 118.5 . . ?
Mo5 O13 Mo6 121.65(13) . . ?
Mo4 O15 Mo5 119.17(12) 2_656 . ?
O1 Co2 O5W 167.70(9) 2_756 . y
O3 Co2 O1 105.11(9) . 2_756 y
O3 Co2 O5W 84.41(9) . . y
O3 Co2 N1 76.94(9) . . y
O3W Co2 O1 82.66(10) . 2_756 y
O3W Co2 O3 91.74(11) . . y
O3W Co2 O5W 89.37(11) . . y
O3W Co2 N1 161.92(12) . . y
O4W Co2 O1 84.22(10) . 2_756 y
O4W Co2 O3 168.03(10) . . y
O4W Co2 O3W 96.97(12) . . y
O4W Co2 O5W 87.47(9) . . y
O4W Co2 N1 96.46(11) . . y
N1 Co2 O1 86.71(9) . 2_756 y
N1 Co2 O5W 103.27(10) . . y
C7 O1 Co2 140.4(2) . 2_756 ?
C1 O3 Co2 118.36(18) . . ?
Co2 O3W H3WA 111.6 . . ?
Co2 O3W H3WB 111.4 . . ?
H3WA O3W H3WB 102.3 . . ?
Co2 O4W H4WA 110.8 . . ?
Co2 O4W H4WB 110.3 . . ?
H4WA O4W H4WB 102.9 . . ?
Co2 O5W H5WA 125.3 . . ?
Co2 O5W H5WB 79.4 . . ?
H5WA O5W H5WB 141.5 . . ?
C2 N1 Co2 114.34(19) . . ?
C6 N1 Co2 126.4(2) . . ?
C6 N1 C2 118.7(3) . . ?
C7 N2 H2 116.4 . . ?
C7 N2 C8 127.2(3) . . ?
C8 N2 H2 116.4 . . ?
C11 N3 H3 118.4 . . ?
C11 N3 C12 123.2(3) . . ?
C12 N3 H3 118.4 . . ?
O2 C1 O3 126.2(3) . . ?
O2 C1 C2 118.4(3) . . ?
O3 C1 C2 115.5(3) . . ?
N1 C2 C1 114.4(3) . . ?
N1 C2 C3 122.4(3) . . ?
C3 C2 C1 123.1(3) . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 C7 124.8(3) . . ?
C4 C3 C7 116.8(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
N1 C6 C5 122.2(3) . . ?
N1 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
O1 C7 N2 123.8(3) . . ?
O1 C7 C3 120.7(3) . . ?
N2 C7 C3 115.3(3) . . ?
C9 C8 N2 124.5(3) . . ?
C9 C8 C12 118.6(3) . . ?
C12 C8 N2 116.8(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
N3 C11 C10 119.1(3) . . ?
N3 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
N3 C12 C8 119.4(3) . . ?
N3 C12 H12 120.3 . . ?
C8 C12 H12 120.3 . . ?
H6WA O6W H6WB 104.5 . . ?
H7WA O7W H7WB 104.5 . . ?
H8WA O8W H8WB 104.6 . . ?
H10B O10W H10C 103.8(16) . . ?
C16 O29 H29 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
O29 C16 C15 102.4(11) . . ?
O29 C16 H16A 111.3 . . ?
O29 C16 H16B 111.3 . . ?
C15 C16 H16A 111.3 . . ?
C15 C16 H16B 111.3 . . ?
H16A C16 H16B 109.2 . . ?
C13 O30 H30 109.5 . . ?
O30 C13 H13A 101.8 . . ?
O30 C13 H13B 101.8 . . ?
O30 C13 C14 140.8(15) . . ?
H13A C13 H13B 104.7 . . ?
C14 C13 H13A 101.8 . . ?
C14 C13 H13B 101.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O18 Mo3 O28 Co1 -103.9(9) 2_767 . . . ?
O23 Mo3 O28 Co1 155.4(7) . . . . ?
O25 Mo3 O28 Co1 102.5(9) . . . . ?
O26 Mo3 O28 Co1 -1.4(9) . . . . ?
O27 Mo3 O28 Co1 -174.9(9) . . . . ?
O9 Mo5 O13 Mo6 -88.36(15) 2_656 . . . ?
O12 Mo5 O13 Mo6 -17.57(13) . . . . ?
O14 Mo5 O13 Mo6 76.07(18) . . . . ?
O15 Mo5 O13 Mo6 -45.0(3) . . . . ?
O16 Mo5 O13 Mo6 -177.33(17) . . . . ?
Co2 O1 C7 N2 -179.3(2) 2_756 . . . ?
Co2 O1 C7 C3 5.7(5) 2_756 . . . ?
Co2 O3 C1 O2 172.7(2) . . . . ?
Co2 O3 C1 C2 -6.1(3) . . . . ?
Co2 N1 C2 C1 3.8(3) . . . . ?
Co2 N1 C2 C3 -172.8(2) . . . . ?
Co2 N1 C6 C5 170.2(2) . . . . ?
O2 C1 C2 N1 -177.6(3) . . . . ?
O2 C1 C2 C3 -1.0(4) . . . . ?
O3 C1 C2 N1 1.3(4) . . . . ?
O3 C1 C2 C3 177.9(3) . . . . ?
N1 C2 C3 C4 2.2(4) . . . . ?
N1 C2 C3 C7 -179.3(3) . . . . ?
N2 C8 C9 C10 -178.9(4) . . . . ?
N2 C8 C12 N3 179.6(3) . . . . ?
C1 C2 C3 C4 -174.1(3) . . . . ?
C1 C2 C3 C7 4.4(4) . . . . ?
C2 N1 C6 C5 -0.9(5) . . . . ?
C2 C3 C4 C5 -2.1(4) . . . . ?
C2 C3 C7 O1 -109.3(4) . . . . ?
C2 C3 C7 N2 75.2(4) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C4 C3 C7 O1 69.2(4) . . . . ?
C4 C3 C7 N2 -106.2(3) . . . . ?
C4 C5 C6 N1 0.9(5) . . . . ?
C6 N1 C2 C1 175.9(3) . . . . ?
C6 N1 C2 C3 -0.7(4) . . . . ?
C7 N2 C8 C9 -13.8(5) . . . . ?
C7 N2 C8 C12 168.2(3) . . . . ?
C7 C3 C4 C5 179.2(3) . . . . ?
C8 N2 C7 O1 1.1(5) . . . . ?
C8 N2 C7 C3 176.4(3) . . . . ?
C8 C9 C10 C11 -0.8(7) . . . . ?
C9 C8 C12 N3 1.4(5) . . . . ?
C9 C10 C11 N3 2.1(7) . . . . ?
C11 N3 C12 C8 -0.1(5) . . . . ?
C12 N3 C11 C10 -1.7(6) . . . . ?
C12 C8 C9 C10 -0.9(5) . . . . ?
_iucr_refine_instructions_details
;
5.res created by SHELXL-2014/7
TITL 1 in P-1
CELL 0.71073 12.3636 13.0466 14.4949 106.06 97.818 111.813
ZERR 1 0.0005 0.0005 0.0005 0.001 0.001 0.001
LATT 1
SFAC C H Co Cr Mo N O
UNIT 28 76 3 2 12 6 73
DFIX 1.52 C16 C15 C13 C14
DFIX 1.42 C16 O29 O30 C13
DFIX 0.85 0.001 H10b O10W
DFIX 0.85 0.001 O10W H10c
DFIX 1.402 O30 C13 C16 O29
DFIX 1.389 H10c H10b
DFIX 1.52 C13 C14
DANG 2.52 C15 O29 C14 O30
DELU O29 > C14
SIMU 0.01 0.01 2 O29 > C14
L.S. 20
PLAN 50
LIST 1
bump
conf
Htab
bond $H
fmap 2
acta
MERG 2
OMIT 1 -1 2
OMIT 1 9 0
OMIT -11 7 5
OMIT 2 -1 2
OMIT -5 5 0
OMIT -2 -4 3
OMIT -5 2 3
OMIT 4 -4 3
OMIT 11 -2 3
OMIT -1 -5 3
OMIT -2 -1 4
OMIT -1 -2 3
OMIT -4 2 3
OMIT -1 0 2
OMIT -5 2 1
OMIT -4 4 0
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.036500 2.667600
FVAR 0.87266
MO1 5 1.172471 0.591166 0.852184 11.00000 0.02184 0.01923 =
0.01852 0.00749 0.00796 0.00861
MO2 5 1.205905 0.400062 0.950751 11.00000 0.02239 0.02533 =
0.02232 0.01014 0.00795 0.01549
MO3 5 0.960536 0.684278 0.895123 11.00000 0.03433 0.02511 =
0.02485 0.01575 0.01365 0.02034
CO1 3 1.000000 1.000000 1.000000 10.50000 0.04562 0.02446 =
0.03365 0.01426 0.01489 0.02333
CR1 4 1.000000 0.500000 1.000000 10.50000 0.01486 0.01385 =
0.01231 0.00495 0.00280 0.00736
O1W 7 1.172829 1.059239 1.089133 11.00000 0.06616 0.07444 =
0.04660 0.01004 -0.00244 0.03963
AFIX 7
H1WA 2 1.190969 1.022730 1.134284 11.00000 -1.50000
H1WB 2 1.217610 1.136340 1.138752 11.00000 -1.50000
AFIX 0
O2W 7 1.072724 1.024135 0.884823 11.00000 0.06617 0.03743 =
0.04619 0.02323 0.02586 0.03239
AFIX 7
H2WA 2 1.128868 0.995654 0.877930 11.00000 -1.50000
H2WB 2 1.116757 1.101237 0.895841 11.00000 -1.50000
AFIX 0
O17 7 1.178599 0.255750 0.894570 11.00000 0.05340 0.03570 =
0.03554 0.01666 0.02160 0.03074
O18 7 1.193731 0.402260 1.085012 11.00000 0.02751 0.03556 =
0.02466 0.01442 0.00862 0.02074
O19 7 1.156981 0.434296 0.836368 11.00000 0.02911 0.02211 =
0.01966 0.00679 0.00942 0.01388
O20 7 1.358771 0.476971 0.983354 11.00000 0.02525 0.05466 =
0.04148 0.02203 0.01167 0.02036
O21 7 1.129529 0.572104 0.728537 11.00000 0.03913 0.02798 =
0.02425 0.01248 0.01093 0.01368
O22 7 1.324569 0.671530 0.889553 11.00000 0.02589 0.03395 =
0.03819 0.01035 0.01064 0.00751
O23 7 0.976925 0.512359 0.867012 11.00000 0.01876 0.01739 =
0.01429 0.00519 0.00215 0.00731
AFIX 13
H23 2 0.916159 0.442953 0.811368 11.00000 -1.20000
AFIX 0
O24 7 1.173550 0.566757 1.004329 11.00000 0.01633 0.01871 =
0.01608 0.00384 0.00218 0.00644
AFIX 13
H24 2 1.230779 0.632265 1.064395 11.00000 -1.20000
AFIX 0
O25 7 1.128688 0.716312 0.912054 11.00000 0.03151 0.01663 =
0.03162 0.00973 0.01477 0.00961
O26 7 0.915115 0.657237 0.772097 11.00000 0.05906 0.07080 =
0.03287 0.03396 0.01828 0.04130
O27 7 0.992707 0.653390 1.044821 11.00000 0.02117 0.01576 =
0.02124 0.00490 0.00477 0.00882
AFIX 13
H27 2 1.056374 0.717663 1.102229 11.00000 -1.20000
AFIX 0
O28 7 0.982691 0.826804 0.955314 11.00000 0.05962 0.02856 =
0.06001 0.02570 0.03439 0.03027
MO4 5 0.394858 -0.284260 0.468376 11.00000 0.02206 0.01389 =
0.04972 0.00699 0.01555 0.00661
MO5 5 0.666352 0.205139 0.723352 11.00000 0.02447 0.01728 =
0.03882 -0.00321 0.01383 0.00322
MO6 5 0.546124 -0.082383 0.694943 11.00000 0.02608 0.02315 =
0.04363 0.01187 0.01627 0.00885
CR2 4 0.500000 0.000000 0.500000 10.50000 0.01747 0.01163 =
0.03490 0.00338 0.01318 0.00477
O4 7 0.479603 -0.358580 0.486120 11.00000 0.03210 0.02732 =
0.07012 0.01458 0.01834 0.01718
O5 7 0.248326 -0.387616 0.433569 11.00000 0.02708 0.02272 =
0.06784 0.01156 0.01670 0.00637
O6 7 0.394628 -0.206831 0.604618 11.00000 0.02549 0.02237 =
0.05062 0.01398 0.02007 0.00595
O8 7 0.497236 -0.052159 0.798937 11.00000 0.04581 0.05318 =
0.04874 0.01820 0.02482 0.01897
O9 7 0.343748 -0.140336 0.442136 11.00000 0.01800 0.01431 =
0.03851 0.00307 0.01438 0.00519
AFIX 13
H9A 2 0.272631 -0.134479 0.461270 11.00000 -1.20000
AFIX 0
O10 7 0.559838 -0.108220 0.534446 11.00000 0.01969 0.01567 =
0.04219 0.00732 0.01670 0.00670
AFIX 13
H10A 2 0.635985 -0.105344 0.520289 11.00000 -1.20000
AFIX 0
O11 7 0.628373 -0.158255 0.712548 11.00000 0.03628 0.03086 =
0.06728 0.02055 0.01360 0.01294
O12 7 0.484642 0.041136 0.638559 11.00000 0.02024 0.01918 =
0.04070 0.00473 0.01742 0.00762
AFIX 13
H12A 2 0.409793 0.045268 0.649969 11.00000 -1.20000
AFIX 0
O13 7 0.685174 0.067599 0.724211 11.00000 0.02469 0.02286 =
0.04843 0.00539 0.01444 0.00715
O14 7 0.630997 0.245749 0.834099 11.00000 0.04182 0.03910 =
0.04127 0.00224 0.01925 0.01779
O15 7 0.583830 0.275794 0.658016 11.00000 0.02954 0.01829 =
0.04666 -0.00045 0.01730 0.00947
O16 7 0.815733 0.298803 0.747840 11.00000 0.02797 0.02385 =
0.05602 -0.00294 0.01197 0.00035
CO2 3 0.974879 0.243528 0.469538 11.00000 0.01957 0.01953 =
0.02215 0.00873 0.00724 0.00808
O1 7 0.866495 -0.279732 0.415015 11.00000 0.02378 0.02649 =
0.02704 0.01220 -0.00198 0.00893
O2 7 0.750700 -0.083819 0.464340 11.00000 0.02798 0.02287 =
0.03838 0.01072 0.02029 0.00929
O3 7 0.831816 0.108557 0.485632 11.00000 0.02380 0.02041 =
0.03118 0.00941 0.01483 0.01131
O3W 7 0.959024 0.367065 0.579442 11.00000 0.02660 0.04246 =
0.04619 -0.01093 0.00227 0.01582
AFIX 7
H3WA 2 0.898782 0.383978 0.558065 11.00000 -1.50000
H3WB 2 1.023141 0.436576 0.598905 11.00000 -1.50000
AFIX 0
O4W 7 1.097309 0.355992 0.423253 11.00000 0.02671 0.04210 =
0.03848 0.02758 0.01037 0.00987
AFIX 7
H4WA 2 1.074518 0.336341 0.358383 11.00000 -1.50000
H4WB 2 1.165251 0.348759 0.432566 11.00000 -1.50000
AFIX 0
O5W 7 0.831709 0.248880 0.362084 11.00000 0.02036 0.03310 =
0.03739 0.01750 0.00708 0.00910
AFIX 3
H5WA 2 0.756799 0.220720 0.359364 11.00000 -1.20000
H5WB 2 0.882549 0.303720 0.368854 11.00000 -1.20000
AFIX 0
N1 6 0.991158 0.088974 0.388736 11.00000 0.01794 0.02052 =
0.02082 0.00800 0.00482 0.00657
N2 6 0.722527 -0.284273 0.295908 11.00000 0.02109 0.01812 =
0.02125 0.00782 0.00196 0.00850
AFIX 43
H2 2 0.708487 -0.245204 0.260501 11.00000 -1.20000
AFIX 0
N3 6 0.421616 -0.521890 0.205602 11.00000 0.02006 0.03139 =
0.03081 0.00849 -0.00027 0.00789
AFIX 43
H3 2 0.352238 -0.535853 0.170711 11.00000 -1.20000
AFIX 0
C1 1 0.823153 0.003609 0.452383 11.00000 0.01729 0.02180 =
0.01807 0.00722 0.00509 0.00844
C2 1 0.912603 -0.011641 0.395012 11.00000 0.01473 0.02179 =
0.01573 0.00639 0.00339 0.00728
C3 1 0.918411 -0.118473 0.356548 11.00000 0.01797 0.02380 =
0.01440 0.00638 0.00268 0.00914
C4 1 1.012252 -0.120609 0.312546 11.00000 0.02405 0.02635 =
0.02205 0.00646 0.00730 0.01418
AFIX 43
H4 2 1.020418 -0.190399 0.287939 11.00000 -1.20000
AFIX 0
C5 1 1.091823 -0.017599 0.306527 11.00000 0.02068 0.03629 =
0.02757 0.01061 0.01136 0.01468
AFIX 43
H5 2 1.154210 -0.017066 0.277048 11.00000 -1.20000
AFIX 0
C6 1 1.078511 0.085458 0.344656 11.00000 0.02134 0.02912 =
0.02962 0.01160 0.01244 0.00886
AFIX 43
H6 2 1.132160 0.154503 0.339401 11.00000 -1.20000
AFIX 0
C7 1 0.832637 -0.233573 0.360318 11.00000 0.02197 0.02100 =
0.01712 0.00454 0.00552 0.01044
C8 1 0.628170 -0.393662 0.280093 11.00000 0.02055 0.01917 =
0.01821 0.00539 0.00442 0.00839
C9 1 0.641081 -0.478999 0.314163 11.00000 0.02517 0.02799 =
0.04005 0.01489 0.00029 0.00942
AFIX 43
H9 2 0.715979 -0.465148 0.351185 11.00000 -1.20000
AFIX 0
C10 1 0.541641 -0.584805 0.292600 11.00000 0.03742 0.03051 =
0.06378 0.02801 0.00072 0.00767
AFIX 43
H10 2 0.549818 -0.642849 0.314451 11.00000 -1.20000
AFIX 0
C11 1 0.430900 -0.604470 0.239056 11.00000 0.02900 0.03026 =
0.05088 0.01804 0.00087 0.00190
AFIX 43
H11 2 0.363244 -0.674487 0.226290 11.00000 -1.20000
AFIX 0
C12 1 0.514955 -0.418294 0.223635 11.00000 0.02414 0.02567 =
0.02478 0.00950 0.00260 0.01178
AFIX 43
H12 2 0.504351 -0.363219 0.198702 11.00000 -1.20000
AFIX 6
O6W 7 1.183910 0.859158 1.104568 10.50000 0.06727 0.06148 =
0.05895 0.00745 -0.00436 0.02688
H6WA 2 1.226232 0.837283 1.069051 10.50000 -1.50000
H6WB 2 1.227409 0.886258 1.164135 10.50000 -1.50000
AFIX 6
O7W 7 1.322049 0.392029 0.434424 11.00000 0.03473 0.04877 =
0.10788 0.03844 0.01844 0.01953
H7WA 2 1.367190 0.465371 0.464181 11.00000 -1.50000
H7WB 2 1.363376 0.358115 0.452672 11.00000 -1.50000
AFIX 6
O8W 7 1.226066 0.936475 0.825640 11.00000 0.06603 0.04918 =
0.08375 0.02135 0.04154 0.03073
H8WA 2 1.172199 0.871631 0.782866 11.00000 -1.50000
H8WB 2 1.291788 0.929752 0.826198 11.00000 -1.50000
AFIX 0
O10W 7 0.353229 0.123122 0.769649 11.00000 0.04495 0.06884 =
0.07305 0.04609 0.02333 0.03458
H10B 2 0.295479 0.117092 0.796797 11.00000 0.26502
H10C 2 0.385107 0.083627 0.791003 11.00000 0.41618
PART 1
O29 7 0.394724 -0.085923 1.000405 10.50000 0.12999 0.09991 =
0.10480 -0.00473 0.00236 0.01854
AFIX 83
H29 2 0.379608 -0.145784 1.014157 10.50000 -1.50000
AFIX 0
C15 1 0.372491 0.075498 1.018209 10.50000 0.09246 0.10195 =
0.08290 0.01263 -0.00144 0.00105
AFIX 137
H15A 2 0.456938 0.108613 1.051443 10.50000 -1.50000
H15B 2 0.335262 0.118981 1.055781 10.50000 -1.50000
H15C 2 0.363274 0.080024 0.952812 10.50000 -1.50000
AFIX 0
C16 1 0.312003 -0.053631 1.009597 10.50000 0.06680 0.06056 =
0.04206 0.00997 -0.00401 0.01093
AFIX 23
H16A 2 0.286597 -0.060574 1.068890 10.50000 -1.20000
H16B 2 0.242605 -0.099368 0.951835 10.50000 -1.20000
AFIX 0
PART 0
PART 2
O30 7 0.452573 0.285574 0.965095 10.50000 0.02551 0.05181 =
0.06576 0.00269 0.00000 0.01835
AFIX 83
H30 2 0.449908 0.238446 0.912894 10.50000 -1.50000
AFIX 0
C13 1 0.391236 0.227798 1.015890 10.50000 0.08661 0.10013 =
0.09471 0.00264 -0.00626 0.01400
AFIX 23
H13A 2 0.312296 0.180543 0.968475 10.50000 -1.20000
H13B 2 0.381180 0.289572 1.064176 10.50000 -1.20000
AFIX 0
C14 1 0.396508 0.152410 1.071031 10.50000 0.10388 0.11048 =
0.09574 0.01674 0.00192 -0.00219
AFIX 137
H14A 2 0.325656 0.078484 1.042340 10.50000 -1.50000
H14B 2 0.400151 0.189994 1.139175 10.50000 -1.50000
H14C 2 0.467225 0.138556 1.068291 10.50000 -1.50000
AFIX 0
HKLF 4
REM 1 in P-1
REM R1 = 0.0283 for 8622 Fo > 4sig(Fo) and 0.0343 for all 9866 data
REM 618 parameters refined using 70 restraints
END
WGHT 0.0366 2.6514
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, -y+1, -z+2
HTAB O1W O11_$1
HTAB O1W O6W
HTAB O1W O11_$1
HTAB O2W O8W
EQIV $2 x, y+1, z
HTAB O2W O17_$2
HTAB O23 O16
HTAB O24 O14_$1
HTAB O27 O16_$1
HTAB O27 O6W
EQIV $3 -x+1, -y, -z+1
HTAB O9 O3_$3
HTAB O10 O2
HTAB O12 O10W
HTAB O3W O5_$3
HTAB O3W O21
EQIV $4 -x+2, -y+1, -z+1
HTAB O4W O26_$4
HTAB O4W O7W
HTAB O5W O6_$3
HTAB O5W O21_$4
HTAB O5W O4W
HTAB N2 O10W_$3
EQIV $5 x-1, y-1, z-1
HTAB N3 O18_$5
EQIV $6 -x+2, -y, -z+1
HTAB C5 O13_$6
HTAB C9 O1
EQIV $7 -x+1, -y-1, -z+1
HTAB C10 O11_$7
HTAB C11 O11_$7
HTAB O6W O25
EQIV $8 x+1, y+1, z
HTAB O6W O29_$8
HTAB O6W O13_$1
HTAB O7W O4_$8
HTAB O7W O4_$6
HTAB O8W O5W_$4
HTAB O8W O8_$8
HTAB O10W O8
EQIV $9 x-1, y-1, z
HTAB O29 O22_$9
EQIV $10 -x+1, -y, -z+2
HTAB C15 O8_$10
HTAB C15 O29_$10
HTAB C15 O1W_$9
HTAB C15 O8W_$9
HTAB C16 O6W_$9
HTAB C16 O25_$9
HTAB C16 O8W_$9
HTAB O30 O14
HTAB O30 O10W
EQIV $11 x-1, y, z
HTAB C13 O17_$11
EQIV $12 x, y+1, z+1
HTAB C13 N3_$12
HTAB C14 O1W_$9
HTAB C14 O11_$10
REM Highest difference peak 0.893, deepest hole -1.327, 1-sigma level 0.113
Q1 1 0.3857 0.1773 0.8307 11.00000 0.05 0.80
Q2 1 0.4451 0.3038 1.0084 11.00000 0.05 0.71
Q3 1 0.5470 -0.0657 0.5259 11.00000 0.05 0.50
Q4 1 0.5784 -0.1406 0.7059 11.00000 0.05 0.49
Q5 1 1.1770 0.4645 0.9358 11.00000 0.05 0.48
Q6 1 1.2578 0.9473 0.8864 11.00000 0.05 0.48
Q7 1 0.6159 0.2078 0.7069 11.00000 0.05 0.48
Q8 1 0.4259 -0.3420 0.4821 11.00000 0.05 0.46
Q9 1 0.3049 0.0587 0.7852 11.00000 0.05 0.44
Q10 1 1.1300 0.6445 0.8338 11.00000 0.05 0.44
Q11 1 0.6177 0.2594 0.6720 11.00000 0.05 0.44
Q12 1 0.3389 -0.2179 0.4334 11.00000 0.05 0.44
Q13 1 1.1451 0.6563 0.8992 11.00000 0.05 0.43
Q14 1 1.2008 0.5274 0.8573 11.00000 0.05 0.41
Q15 1 0.5049 -0.0624 0.6815 11.00000 0.05 0.41
Q16 1 0.9279 0.7380 0.9164 11.00000 0.05 0.41
Q17 1 1.2382 0.3372 0.9265 11.00000 0.05 0.40
Q18 1 0.8416 0.3331 0.3486 11.00000 0.05 0.38
Q19 1 0.9408 0.7038 0.8034 11.00000 0.05 0.37
Q20 1 0.8773 -0.0073 0.4298 11.00000 0.05 0.37
Q21 1 0.8951 -0.0594 0.3621 11.00000 0.05 0.37
Q22 1 0.6659 0.1600 0.7338 11.00000 0.05 0.36
Q23 1 0.9441 0.0355 0.3734 11.00000 0.05 0.36
Q24 1 1.0346 0.9450 1.0208 11.00000 0.05 0.36
Q25 1 0.9424 0.1783 0.4075 11.00000 0.05 0.35
Q26 1 0.3815 -0.2619 0.5167 11.00000 0.05 0.35
Q27 1 1.0234 0.7917 0.9343 11.00000 0.05 0.35
Q28 1 0.7272 0.1409 0.7387 11.00000 0.05 0.34
Q29 1 0.4978 0.2599 1.0680 11.00000 0.05 0.34
Q30 1 0.9548 0.7798 0.9680 11.00000 0.05 0.34
Q31 1 0.5107 0.3219 1.0210 11.00000 0.05 0.33
Q32 1 1.1454 0.2957 0.8999 11.00000 0.05 0.33
Q33 1 0.3566 -0.2194 0.4958 11.00000 0.05 0.32
Q34 1 0.9813 0.1469 0.4132 11.00000 0.05 0.32
Q35 1 1.0489 0.0210 0.2957 11.00000 0.05 0.32
Q36 1 0.8737 -0.1665 0.3524 11.00000 0.05 0.32
Q37 1 1.3895 0.3767 1.0028 11.00000 0.05 0.32
Q38 1 1.2747 0.4386 0.4465 11.00000 0.05 0.32
Q39 1 0.5369 -0.3377 0.5089 11.00000 0.05 0.32
Q40 1 0.5766 -0.4244 0.2280 11.00000 0.05 0.32
Q41 1 1.2177 1.0271 1.0644 11.00000 0.05 0.31
Q42 1 0.9813 -0.1055 0.3463 11.00000 0.05 0.31
Q43 1 0.9972 0.6207 0.9123 11.00000 0.05 0.31
Q44 1 0.4548 -0.3272 0.5260 11.00000 0.05 0.31
Q45 1 0.6134 0.0283 0.7023 11.00000 0.05 0.31
Q46 1 0.4972 -0.0238 0.6456 11.00000 0.05 0.30
Q47 1 1.1967 0.3635 1.0275 11.00000 0.05 0.30
Q48 1 0.9279 0.7539 0.7794 11.00000 0.05 0.30
Q49 1 0.5323 -0.0744 0.5943 11.00000 0.05 0.30
Q50 1 0.7118 0.1613 0.7859 11.00000 0.05 0.30
REM The information below was added by Olex2.
REM
REM R1 = 0.0283 for 8622 Fo > 4sig(Fo) and 0.0343 for all 14826 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.89, deepest hole -1.33
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0343
REM R1_gt = 0.0283
REM wR_ref = 0.0744
REM GOOF = 1.035
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 14826
REM Reflections_gt = 8622
REM Parameters = n/a
REM Hole = -1.33
REM Peak = 0.89
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_4
_database_code_depnum_ccdc_archive 'CCDC 1540700'
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_4
;
PROBLEM: Short Inter D-H..H-D H6 .. H9WB .. 2.08 Ang.
RESPONSE: This is due to disordered solvate water molecule in the structure.
;
# end Validation Reply Form
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C25 H53 Co3 Cr Mo6 N6 O46'
_chemical_formula_weight 1978.16
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'
Cr Cr 0.3209 0.6236 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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 25.9299(17)
_cell_length_b 9.8335(6)
_cell_length_c 24.7101(16)
_cell_angle_alpha 90
_cell_angle_beta 117.076(2)
_cell_angle_gamma 90
_cell_volume 5610.1(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 3656
_cell_measurement_theta_min 2.25
_cell_measurement_theta_max 27.86
_exptl_crystal_description block
_exptl_crystal_colour green
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 2.342
_exptl_crystal_F_000 3880
_exptl_transmission_factor_min 0.708
_exptl_transmission_factor_max 0.782
_exptl_crystal_size_max 0.170
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.100
_exptl_absorpt_coefficient_mu 2.463
_shelx_estimated_absorpt_T_min 0.680
_shelx_estimated_absorpt_T_max 0.791
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source 'sealed tube'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 19751
_diffrn_reflns_av_unetI/netI 0.0516
_diffrn_reflns_av_R_equivalents 0.0444
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 1.851
_diffrn_reflns_theta_max 28.005
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 6756
_reflns_number_gt 5127
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'SAINT v8.34A (Bruker, 2013)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.6187P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6756
_refine_ls_number_parameters 442
_refine_ls_number_restraints 13
_refine_ls_R_factor_all 0.0551
_refine_ls_R_factor_gt 0.0340
_refine_ls_wR_factor_ref 0.0717
_refine_ls_wR_factor_gt 0.0653
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_restrained_S_all 1.013
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.50343(2) 0.73454(3) 0.40520(2) 0.01837(8) Uani 1 1 d . . . . .
Mo2 Mo 0.61844(2) 0.68734(3) 0.53706(2) 0.01851(8) Uani 1 1 d . . . . .
Mo3 Mo 0.61247(2) 0.45712(3) 0.63417(2) 0.01871(8) Uani 1 1 d . . . . .
Co1 Co 0.5000 0.73324(8) 0.2500 0.02079(17) Uani 1 2 d S T P . .
Co2 Co 0.71300(2) 0.22452(6) 0.61477(2) 0.02288(13) Uani 1 1 d . . . . .
Cr1 Cr 0.5000 0.5000 0.5000 0.01597(18) Uani 1 2 d S . P . .
O1 O 0.75548(11) 0.4581(3) 0.40648(12) 0.0295(7) Uani 1 1 d . . . . .
O1W O 0.77482(13) 0.1813(4) 0.70272(13) 0.0421(8) Uani 1 1 d . . . . .
H1WA H 0.7594 0.1365 0.7214 0.063 Uiso 1 1 d R U . . .
H1WB H 0.7859 0.2556 0.7227 0.063 Uiso 1 1 d R U . . .
O2 O 0.65553(11) 0.3703(3) 0.44179(12) 0.0324(7) Uani 1 1 d . . . . .
O2W O 0.65311(11) 0.0923(3) 0.62161(13) 0.0297(7) Uani 1 1 d . . . . .
H2WA H 0.6391 0.0354 0.5912 0.045 Uiso 1 1 d R U . . .
H2WB H 0.6224 0.1371 0.6176 0.045 Uiso 1 1 d R U . . .
O3 O 0.65859(11) 0.2726(3) 0.52468(12) 0.0262(6) Uani 1 1 d . . . . .
O3W O 0.5000 0.5197(5) 0.2500 0.0451(12) Uani 1 2 d S T P . .
H3WA H 0.4825 0.4859 0.2125 0.068 Uiso 0.5 1 d R U P . .
H3WB H 0.4786 0.4859 0.2666 0.068 Uiso 0.5 1 d R U P . .
O4 O 0.67787(11) 0.3864(3) 0.64434(12) 0.0252(6) Uani 1 1 d . . . . .
O4W O 0.5000 0.9475(4) 0.2500 0.0401(11) Uani 1 2 d S T P . .
H4WA H 0.4779 0.9792 0.2652 0.060 Uiso 0.5 1 d R U P . .
H4WB H 0.4838 0.9792 0.2129 0.060 Uiso 0.5 1 d R U P . .
O5 O 0.62028(12) 0.4847(3) 0.70507(12) 0.0314(7) Uani 1 1 d . . . . .
O6 O 0.51969(10) 0.4833(3) 0.58735(11) 0.0213(6) Uani 1 1 d . . . . .
H6 H 0.5034 0.5525 0.6037 0.026 Uiso 0.8333 1 calc R U P . .
O7 O 0.61986(11) 0.6432(3) 0.61445(11) 0.0230(6) Uani 1 1 d . . . . .
O8 O 0.58379(10) 0.4714(3) 0.53056(10) 0.0174(5) Uani 1 1 d . . . . .
H8 H 0.5969 0.4011 0.5115 0.021 Uiso 0.8333 1 calc R U P . .
O9 O 0.68430(11) 0.6310(3) 0.54737(12) 0.0307(7) Uani 1 1 d . . . . .
O10 O 0.62565(12) 0.8595(3) 0.54785(13) 0.0308(7) Uani 1 1 d . . . . .
O11 O 0.52000(10) 0.6941(3) 0.50245(11) 0.0180(5) Uani 1 1 d . . . . .
H11 H 0.5043 0.7582 0.5215 0.022 Uiso 0.8333 1 calc R U P . .
O12 O 0.58194(10) 0.6739(3) 0.44996(11) 0.0207(6) Uani 1 1 d . . . . .
O13 O 0.51131(12) 0.9041(3) 0.42048(13) 0.0328(7) Uani 1 1 d . . . . .
O14 O 0.42292(11) 0.7255(3) 0.38480(12) 0.0234(6) Uani 1 1 d . . . . .
O15 O 0.50026(11) 0.7194(3) 0.33419(11) 0.0262(6) Uani 1 1 d . . . . .
N1 N 0.59195(13) 0.7402(4) 0.29185(14) 0.0252(8) Uani 1 1 d . . . . .
N2 N 0.71238(13) 0.6238(3) 0.43381(14) 0.0257(8) Uani 1 1 d . . . . .
H2 H 0.7090 0.6626 0.4632 0.031 Uiso 1 1 calc R U . . .
N3 N 0.76691(13) 0.3498(4) 0.59293(14) 0.0247(7) Uani 1 1 d . . . . .
C1 C 0.62130(17) 0.7940(5) 0.26387(17) 0.0284(10) Uani 1 1 d . . . . .
H1 H 0.6005 0.8363 0.2264 0.034 Uiso 1 1 calc R U . . .
C2 C 0.68007(17) 0.7893(5) 0.28792(19) 0.0327(10) Uani 1 1 d . . . . .
H2A H 0.6985 0.8256 0.2666 0.039 Uiso 1 1 calc R U . . .
C3 C 0.71229(17) 0.7301(5) 0.34437(19) 0.0318(10) Uani 1 1 d . . . . .
H3 H 0.7524 0.7246 0.3614 0.038 Uiso 1 1 calc R U . . .
C4 C 0.68286(16) 0.6799(4) 0.37436(17) 0.0232(8) Uani 1 1 d . . . . .
C5 C 0.62288(16) 0.6853(4) 0.34651(17) 0.0249(9) Uani 1 1 d . . . . .
H5 H 0.6034 0.6491 0.3668 0.030 Uiso 1 1 calc R U . . .
C6 C 0.74550(15) 0.5116(4) 0.44537(17) 0.0205(8) Uani 1 1 d . . . . .
C7 C 0.77210(15) 0.4655(4) 0.51025(17) 0.0217(8) Uani 1 1 d . . . . .
C8 C 0.82932(16) 0.5032(4) 0.54897(18) 0.0279(9) Uani 1 1 d . . . . .
H8A H 0.8505 0.5546 0.5345 0.033 Uiso 1 1 calc R U . . .
C9 C 0.85349(17) 0.4633(5) 0.60853(19) 0.0339(11) Uani 1 1 d . . . . .
H9 H 0.8916 0.4866 0.6348 0.041 Uiso 1 1 calc R U . . .
C10 C 0.82155(17) 0.3891(5) 0.62928(18) 0.0314(10) Uani 1 1 d . . . . .
H10 H 0.8383 0.3648 0.6701 0.038 Uiso 1 1 calc R U . . .
C11 C 0.74234(15) 0.3875(4) 0.53412(16) 0.0193(8) Uani 1 1 d . . . . .
C12 C 0.68030(15) 0.3404(4) 0.49603(18) 0.0220(8) Uani 1 1 d . . . . .
O5W O 0.468(3) 1.104(7) 0.3222(16) 0.099(10) Uani 0.5 1 d . U P A 2
O6W O 0.3508(2) 1.1588(6) 0.2983(2) 0.110(2) Uani 1 1 d G . . . .
H6WA H 0.3527 1.2285 0.3195 0.164 Uiso 1 1 d G U . . .
H6WB H 0.3856 1.1309 0.3128 0.164 Uiso 1 1 d G U . . .
O7W O 0.2605(5) 1.0387(14) 0.2624(5) 0.107(4) Uani 0.5 1 d G . P . .
H7WA H 0.2492 1.0309 0.2244 0.161 Uiso 0.5 1 d G U P . .
H7WB H 0.2958 1.0622 0.2768 0.161 Uiso 0.5 1 d G U P . .
O8W O 0.45280(15) 0.8424(4) 0.5339(2) 0.0607(11) Uani 1 1 d G . . . .
H8WA H 0.4577 0.9252 0.5449 0.091 Uiso 1 1 d G U . . .
H8WB H 0.4170 0.8226 0.5188 0.091 Uiso 1 1 d G U . . .
O9W O 0.4666(2) 0.6320(4) 0.64163(19) 0.0517(9) Uani 1 1 d D . . . .
H9WA H 0.4314(7) 0.636(8) 0.620(3) 0.11(3) Uiso 1 1 d D . . . .
H9WB H 0.4918(15) 0.685(6) 0.663(3) 0.12(3) Uiso 1 1 d D . . . .
O10W O 0.6182(6) 0.6394(12) 0.8004(7) 0.120(4) Uani 0.5 1 d G . P . .
H10A H 0.6036 0.5927 0.8189 0.180 Uiso 0.5 1 d G U P . .
H10B H 0.6099 0.5952 0.7679 0.180 Uiso 0.5 1 d G U P . .
O16 O 0.478(3) 1.118(7) 0.3232(16) 0.094(8) Uani 0.5 1 d D U P B 1
C13 C 0.4451(7) 1.158(2) 0.2763(7) 0.122(7) Uani 0.5 1 d D . P B 1
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
Mo1 0.02260(17) 0.01841(18) 0.01700(16) 0.00154(13) 0.01153(14) -0.00087(14)
Mo2 0.01903(16) 0.01846(18) 0.01948(17) -0.00285(13) 0.01003(14) -0.00461(13)
Mo3 0.02116(17) 0.01985(18) 0.01652(16) -0.00051(13) 0.00980(14) 0.00071(14)
Co1 0.0192(4) 0.0281(4) 0.0158(4) 0.000 0.0086(3) 0.000
Co2 0.0229(3) 0.0249(3) 0.0229(3) 0.0006(2) 0.0121(2) 0.0013(2)
Cr1 0.0181(4) 0.0171(4) 0.0163(4) -0.0026(3) 0.0110(3) -0.0038(3)
O1 0.0346(16) 0.0316(17) 0.0293(15) 0.0019(13) 0.0206(14) 0.0112(13)
O1W 0.052(2) 0.041(2) 0.0287(17) -0.0010(15) 0.0148(15) -0.0029(17)
O2 0.0261(15) 0.043(2) 0.0252(16) 0.0051(14) 0.0088(13) -0.0015(14)
O2W 0.0273(15) 0.0249(16) 0.0409(17) -0.0036(13) 0.0189(14) 0.0025(13)
O3 0.0223(14) 0.0307(17) 0.0276(15) 0.0005(13) 0.0132(12) -0.0026(12)
O3W 0.073(3) 0.035(3) 0.032(3) 0.000 0.027(3) 0.000
O4 0.0238(14) 0.0247(16) 0.0258(15) 0.0012(12) 0.0101(12) 0.0030(12)
O4W 0.051(3) 0.030(3) 0.050(3) 0.000 0.033(3) 0.000
O5 0.0434(17) 0.0317(18) 0.0218(14) -0.0004(13) 0.0171(14) 0.0023(14)
O6 0.0249(13) 0.0231(15) 0.0195(13) -0.0015(11) 0.0133(12) -0.0019(12)
O7 0.0288(14) 0.0238(15) 0.0176(13) -0.0043(11) 0.0116(12) -0.0019(12)
O8 0.0197(13) 0.0161(14) 0.0175(13) -0.0015(10) 0.0096(11) -0.0015(11)
O9 0.0226(14) 0.0406(19) 0.0306(16) -0.0072(14) 0.0136(13) -0.0038(13)
O10 0.0405(16) 0.0220(16) 0.0352(16) -0.0049(13) 0.0219(14) -0.0102(13)
O11 0.0223(13) 0.0177(14) 0.0191(13) -0.0013(11) 0.0140(11) -0.0011(11)
O12 0.0208(13) 0.0259(15) 0.0189(13) -0.0001(11) 0.0122(11) -0.0013(11)
O13 0.0417(17) 0.0192(16) 0.0376(17) 0.0009(13) 0.0181(14) -0.0024(13)
O14 0.0242(14) 0.0230(15) 0.0267(14) -0.0020(12) 0.0149(12) -0.0008(12)
O15 0.0259(14) 0.0373(18) 0.0191(14) 0.0037(12) 0.0134(12) -0.0003(13)
N1 0.0228(17) 0.033(2) 0.0190(17) 0.0008(15) 0.0088(14) 0.0022(15)
N2 0.0306(18) 0.026(2) 0.0205(17) -0.0011(14) 0.0118(15) 0.0079(15)
N3 0.0237(17) 0.027(2) 0.0233(17) -0.0011(15) 0.0104(14) -0.0001(15)
C1 0.028(2) 0.037(3) 0.018(2) 0.0027(18) 0.0083(18) -0.0032(19)
C2 0.026(2) 0.047(3) 0.028(2) 0.001(2) 0.0145(19) -0.007(2)
C3 0.021(2) 0.043(3) 0.029(2) -0.005(2) 0.0086(18) -0.0053(19)
C4 0.025(2) 0.022(2) 0.0205(19) -0.0010(17) 0.0085(17) 0.0047(17)
C5 0.023(2) 0.031(2) 0.022(2) 0.0005(18) 0.0117(17) 0.0015(18)
C6 0.0171(18) 0.022(2) 0.025(2) 0.0019(17) 0.0114(16) -0.0033(16)
C7 0.0199(19) 0.020(2) 0.024(2) -0.0038(16) 0.0095(16) 0.0013(16)
C8 0.024(2) 0.029(2) 0.032(2) -0.0002(19) 0.0134(19) -0.0025(18)
C9 0.018(2) 0.046(3) 0.030(2) 0.001(2) 0.0039(18) -0.0037(19)
C10 0.028(2) 0.037(3) 0.022(2) 0.0005(19) 0.0063(18) -0.002(2)
C11 0.0196(18) 0.019(2) 0.0193(19) -0.0012(15) 0.0089(16) 0.0024(16)
C12 0.0187(19) 0.021(2) 0.028(2) -0.0037(17) 0.0121(17) 0.0018(16)
O5W 0.133(17) 0.082(12) 0.103(7) -0.022(6) 0.072(7) -0.003(13)
O6W 0.151(5) 0.072(4) 0.055(3) -0.025(3) 0.002(3) 0.041(3)
O7W 0.096(8) 0.119(10) 0.092(8) 0.038(8) 0.030(6) 0.000(7)
O8W 0.044(2) 0.039(2) 0.106(3) -0.038(2) 0.040(2) -0.0102(17)
O9W 0.061(3) 0.054(3) 0.045(2) -0.005(2) 0.029(2) 0.003(2)
O10W 0.160(10) 0.095(9) 0.161(12) -0.054(8) 0.123(10) -0.047(8)
O16 0.130(16) 0.079(11) 0.097(6) -0.014(6) 0.074(7) -0.011(11)
C13 0.162(18) 0.104(16) 0.066(11) 0.008(11) 0.022(12) 0.026(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O13 1.702(3) . ?
Mo1 O15 1.725(2) . ?
Mo1 O14 1.914(2) . ?
Mo1 O12 1.917(2) . ?
Mo1 O6 2.255(3) 5_666 ?
Mo1 O11 2.275(2) . ?
Mo2 O9 1.701(3) . ?
Mo2 O10 1.711(3) . ?
Mo2 O12 1.921(2) . ?
Mo2 O7 1.945(2) . ?
Mo2 O8 2.282(2) . ?
Mo2 O11 2.294(2) . ?
Mo3 O5 1.691(3) . ?
Mo3 O4 1.742(2) . ?
Mo3 O7 1.925(3) . ?
Mo3 O14 1.974(3) 5_666 ?
Mo3 O6 2.158(2) . ?
Mo3 O8 2.323(2) . ?
Co1 O15 2.082(2) . ?
Co1 O15 2.082(2) 2_655 ?
Co1 O3W 2.100(5) . ?
Co1 O4W 2.107(4) . ?
Co1 N1 2.125(3) . ?
Co1 N1 2.125(3) 2_655 ?
Co2 O1W 2.074(3) . ?
Co2 O3 2.076(3) . ?
Co2 O2W 2.090(3) . ?
Co2 N3 2.109(3) . ?
Co2 O4 2.122(3) . ?
Co2 O1 2.135(3) 7_656 ?
Cr1 O8 1.969(2) 5_666 ?
Cr1 O8 1.969(2) . ?
Cr1 O11 1.972(3) 5_666 ?
Cr1 O11 1.972(3) . ?
Cr1 O6 1.986(2) . ?
Cr1 O6 1.986(2) 5_666 ?
O1 C6 1.222(4) . ?
O1 Co2 2.135(3) 7_656 ?
O2 C12 1.230(4) . ?
O3 C12 1.274(5) . ?
O6 Mo1 2.255(3) 5_666 ?
O14 Mo3 1.974(3) 5_666 ?
N1 C5 1.331(5) . ?
N1 C1 1.348(5) . ?
N2 C6 1.347(5) . ?
N2 C4 1.423(5) . ?
N3 C10 1.343(5) . ?
N3 C11 1.346(5) . ?
C1 C2 1.362(5) . ?
C2 C3 1.386(6) . ?
C3 C4 1.375(6) . ?
C4 C5 1.386(5) . ?
C6 C7 1.498(5) . ?
C7 C11 1.395(5) . ?
C7 C8 1.401(5) . ?
C8 C9 1.369(5) . ?
C9 C10 1.367(6) . ?
C11 C12 1.520(5) . ?
O16 C13 1.1500(10) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Mo1 O15 104.81(14) . . ?
O13 Mo1 O14 96.33(12) . . ?
O15 Mo1 O14 100.77(11) . . ?
O13 Mo1 O12 100.85(12) . . ?
O15 Mo1 O12 96.11(11) . . ?
O14 Mo1 O12 151.93(11) . . ?
O13 Mo1 O6 157.33(11) . 5_666 ?
O15 Mo1 O6 96.29(12) . 5_666 ?
O14 Mo1 O6 71.27(10) . 5_666 ?
O12 Mo1 O6 84.79(10) . 5_666 ?
O13 Mo1 O11 89.48(11) . . ?
O15 Mo1 O11 163.28(11) . . ?
O14 Mo1 O11 85.94(10) . . ?
O12 Mo1 O11 72.29(9) . . ?
O6 Mo1 O11 71.18(9) 5_666 . ?
O9 Mo2 O10 105.54(14) . . ?
O9 Mo2 O12 95.42(12) . . ?
O10 Mo2 O12 101.88(12) . . ?
O9 Mo2 O7 102.22(12) . . ?
O10 Mo2 O7 96.66(12) . . ?
O12 Mo2 O7 149.92(11) . . ?
O9 Mo2 O8 92.51(12) . . ?
O10 Mo2 O8 160.58(11) . . ?
O12 Mo2 O8 83.09(10) . . ?
O7 Mo2 O8 72.08(10) . . ?
O9 Mo2 O11 159.44(12) . . ?
O10 Mo2 O11 93.06(11) . . ?
O12 Mo2 O11 71.77(9) . . ?
O7 Mo2 O11 83.86(9) . . ?
O8 Mo2 O11 70.45(9) . . ?
O5 Mo3 O4 105.36(13) . . ?
O5 Mo3 O7 97.51(12) . . ?
O4 Mo3 O7 102.33(12) . . ?
O5 Mo3 O14 102.45(13) . 5_666 ?
O4 Mo3 O14 89.29(12) . 5_666 ?
O7 Mo3 O14 153.34(11) . 5_666 ?
O5 Mo3 O6 96.59(12) . . ?
O4 Mo3 O6 154.07(11) . . ?
O7 Mo3 O6 88.05(10) . . ?
O14 Mo3 O6 72.37(10) 5_666 . ?
O5 Mo3 O8 163.60(11) . . ?
O4 Mo3 O8 89.17(10) . . ?
O7 Mo3 O8 71.48(10) . . ?
O14 Mo3 O8 84.97(10) 5_666 . ?
O6 Mo3 O8 71.48(8) . . ?
O15 Co1 O15 172.50(16) . 2_655 ?
O15 Co1 O3W 86.25(8) . . ?
O15 Co1 O3W 86.25(8) 2_655 . ?
O15 Co1 O4W 93.75(8) . . ?
O15 Co1 O4W 93.75(8) 2_655 . ?
O3W Co1 O4W 180.0 . . ?
O15 Co1 N1 91.33(11) . . ?
O15 Co1 N1 88.91(11) 2_655 . ?
O3W Co1 N1 91.85(10) . . ?
O4W Co1 N1 88.15(10) . . ?
O15 Co1 N1 88.91(11) . 2_655 ?
O15 Co1 N1 91.33(11) 2_655 2_655 ?
O3W Co1 N1 91.85(10) . 2_655 ?
O4W Co1 N1 88.15(10) . 2_655 ?
N1 Co1 N1 176.29(19) . 2_655 ?
O1W Co2 O3 173.75(12) . . ?
O1W Co2 O2W 92.06(12) . . ?
O3 Co2 O2W 93.50(11) . . ?
O1W Co2 N3 95.84(13) . . ?
O3 Co2 N3 78.38(11) . . ?
O2W Co2 N3 170.80(12) . . ?
O1W Co2 O4 92.36(11) . . ?
O3 Co2 O4 90.55(10) . . ?
O2W Co2 O4 89.28(11) . . ?
N3 Co2 O4 95.07(12) . . ?
O1W Co2 O1 83.42(12) . 7_656 ?
O3 Co2 O1 94.44(11) . 7_656 ?
O2W Co2 O1 83.02(11) . 7_656 ?
N3 Co2 O1 93.21(12) . 7_656 ?
O4 Co2 O1 171.05(11) . 7_656 ?
O8 Cr1 O8 180.00(15) 5_666 . ?
O8 Cr1 O11 84.12(10) 5_666 5_666 ?
O8 Cr1 O11 95.88(10) . 5_666 ?
O8 Cr1 O11 95.88(10) 5_666 . ?
O8 Cr1 O11 84.12(10) . . ?
O11 Cr1 O11 180.0 5_666 . ?
O8 Cr1 O6 96.98(10) 5_666 . ?
O8 Cr1 O6 83.02(10) . . ?
O11 Cr1 O6 83.53(10) 5_666 . ?
O11 Cr1 O6 96.47(10) . . ?
O8 Cr1 O6 83.02(10) 5_666 5_666 ?
O8 Cr1 O6 96.98(10) . 5_666 ?
O11 Cr1 O6 96.47(10) 5_666 5_666 ?
O11 Cr1 O6 83.53(10) . 5_666 ?
O6 Cr1 O6 180.0 . 5_666 ?
C6 O1 Co2 142.8(3) . 7_656 ?
C12 O3 Co2 117.3(2) . . ?
Mo3 O4 Co2 142.39(15) . . ?
Cr1 O6 Mo3 105.35(10) . . ?
Cr1 O6 Mo1 102.75(11) . 5_666 ?
Mo3 O6 Mo1 96.64(10) . 5_666 ?
Mo3 O7 Mo2 120.10(13) . . ?
Cr1 O8 Mo2 102.98(11) . . ?
Cr1 O8 Mo3 100.09(9) . . ?
Mo2 O8 Mo3 93.46(9) . . ?
Cr1 O11 Mo1 102.48(10) . . ?
Cr1 O11 Mo2 102.45(10) . . ?
Mo1 O11 Mo2 92.41(8) . . ?
Mo1 O12 Mo2 118.51(12) . . ?
Mo1 O14 Mo3 115.99(13) . 5_666 ?
Mo1 O15 Co1 171.00(18) . . ?
C5 N1 C1 117.4(3) . . ?
C5 N1 Co1 120.3(3) . . ?
C1 N1 Co1 122.2(3) . . ?
C6 N2 C4 121.9(3) . . ?
C10 N3 C11 118.6(3) . . ?
C10 N3 Co2 128.1(3) . . ?
C11 N3 Co2 113.2(2) . . ?
N1 C1 C2 123.0(4) . . ?
C1 C2 C3 119.7(4) . . ?
C4 C3 C2 117.7(4) . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 N2 121.7(3) . . ?
C5 C4 N2 118.8(4) . . ?
N1 C5 C4 122.8(4) . . ?
O1 C6 N2 121.9(4) . . ?
O1 C6 C7 123.5(4) . . ?
N2 C6 C7 114.4(3) . . ?
C11 C7 C8 118.3(4) . . ?
C11 C7 C6 123.0(3) . . ?
C8 C7 C6 118.6(3) . . ?
C9 C8 C7 118.9(4) . . ?
C10 C9 C8 119.8(4) . . ?
N3 C10 C9 122.5(4) . . ?
N3 C11 C7 121.8(3) . . ?
N3 C11 C12 115.6(3) . . ?
C7 C11 C12 122.6(3) . . ?
O2 C12 O3 125.9(3) . . ?
O2 C12 C11 118.8(3) . . ?
O3 C12 C11 115.2(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Mo3 O4 Co2 132.7(2) . . . . ?
O7 Mo3 O4 Co2 -125.8(2) . . . . ?
O14 Mo3 O4 Co2 30.0(2) 5_666 . . . ?
O6 Mo3 O4 Co2 -14.1(4) . . . . ?
O8 Mo3 O4 Co2 -55.0(2) . . . . ?
C5 N1 C1 C2 2.7(6) . . . . ?
Co1 N1 C1 C2 -174.4(3) . . . . ?
N1 C1 C2 C3 -1.7(7) . . . . ?
C1 C2 C3 C4 -1.0(7) . . . . ?
C2 C3 C4 C5 2.5(6) . . . . ?
C2 C3 C4 N2 -176.7(4) . . . . ?
C6 N2 C4 C3 -63.2(6) . . . . ?
C6 N2 C4 C5 117.7(4) . . . . ?
C1 N1 C5 C4 -1.1(6) . . . . ?
Co1 N1 C5 C4 176.1(3) . . . . ?
C3 C4 C5 N1 -1.5(6) . . . . ?
N2 C4 C5 N1 177.7(4) . . . . ?
Co2 O1 C6 N2 -164.6(3) 7_656 . . . ?
Co2 O1 C6 C7 20.2(7) 7_656 . . . ?
C4 N2 C6 O1 5.6(6) . . . . ?
C4 N2 C6 C7 -178.7(3) . . . . ?
O1 C6 C7 C11 -102.5(5) . . . . ?
N2 C6 C7 C11 81.9(5) . . . . ?
O1 C6 C7 C8 78.1(5) . . . . ?
N2 C6 C7 C8 -97.5(4) . . . . ?
C11 C7 C8 C9 -0.5(6) . . . . ?
C6 C7 C8 C9 178.9(4) . . . . ?
C7 C8 C9 C10 -0.7(7) . . . . ?
C11 N3 C10 C9 -1.4(6) . . . . ?
Co2 N3 C10 C9 175.4(3) . . . . ?
C8 C9 C10 N3 1.7(7) . . . . ?
C10 N3 C11 C7 0.2(6) . . . . ?
Co2 N3 C11 C7 -177.1(3) . . . . ?
C10 N3 C11 C12 -179.5(3) . . . . ?
Co2 N3 C11 C12 3.3(4) . . . . ?
C8 C7 C11 N3 0.8(6) . . . . ?
C6 C7 C11 N3 -178.6(4) . . . . ?
C8 C7 C11 C12 -179.6(4) . . . . ?
C6 C7 C11 C12 1.0(6) . . . . ?
Co2 O3 C12 O2 175.3(3) . . . . ?
Co2 O3 C12 C11 -5.3(4) . . . . ?
N3 C11 C12 O2 -179.3(4) . . . . ?
C7 C11 C12 O2 1.1(6) . . . . ?
N3 C11 C12 O3 1.2(5) . . . . ?
C7 C11 C12 O3 -178.4(3) . . . . ?
_refine_diff_density_max 0.697
_refine_diff_density_min -0.657
_refine_diff_density_rms 0.124
_shelx_res_file
;
111.res created by SHELXL-2014/7
TITL 111_a.res in C2/c
REM Old TITL 111 in C2/c
REM SHELXT solution in C2/c
REM R1 0.123, Rweak 0.004, Alpha 0.035, Orientation as input
REM Formula found by SHELXT: C26 N21 O27 Cu10
CELL 0.71073 25.9299 9.8335 24.7101 90 117.076 90
ZERR 4 0.0017 0.0006 0.0016 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Co Cr Mo N O
UNIT 100 212 12 4 24 24 184
SIZE 0.17 0.12 0.1
DFIX 1.15 0.001 O16 C13
DFIX 0.82 0.01 O9W H9Wb H9Wa O9W
DELU O5W O16
SIMU 0.01 0.01 2 O5W O16
L.S. 14
PLAN 20
SIZE 0.1 0.12 0.17
TEMP 23
conf
htab
bump
list 4
fmap 2
acta
OMIT -8 2 7
OMIT 6 2 3
OMIT 2 0 0
OMIT 4 2 6
OMIT -8 2 5
OMIT -9 3 6
OMIT -7 3 8
REM
REM
REM
WGHT 0.028700 0.618700
FVAR 0.09564
MO1 5 0.503426 0.734536 0.405200 11.00000 0.02260 0.01841 =
0.01700 0.00154 0.01153 -0.00087
MO2 5 0.618438 0.687337 0.537063 11.00000 0.01903 0.01846 =
0.01948 -0.00285 0.01003 -0.00461
MO3 5 0.612471 0.457122 0.634169 11.00000 0.02116 0.01985 =
0.01652 -0.00051 0.00980 0.00071
CO1 3 0.500000 0.733236 0.250000 10.50000 0.01918 0.02814 =
0.01580 0.00000 0.00862 0.00000
CO2 3 0.713002 0.224524 0.614766 11.00000 0.02285 0.02490 =
0.02287 0.00056 0.01214 0.00130
CR1 4 0.500000 0.500000 0.500000 10.50000 0.01811 0.01714 =
0.01632 -0.00256 0.01103 -0.00383
O1 7 0.755481 0.458102 0.406475 11.00000 0.03460 0.03158 =
0.02933 0.00191 0.02062 0.01122
O1W 7 0.774819 0.181260 0.702716 11.00000 0.05221 0.04134 =
0.02866 -0.00099 0.01475 -0.00285
AFIX 7
H1WA 2 0.759428 0.136546 0.721431 11.00000 -1.50000
H1WB 2 0.785932 0.255561 0.722742 11.00000 -1.50000
AFIX 0
O2 7 0.655532 0.370282 0.441792 11.00000 0.02614 0.04254 =
0.02524 0.00508 0.00878 -0.00148
O2W 7 0.653110 0.092318 0.621607 11.00000 0.02728 0.02492 =
0.04088 -0.00358 0.01885 0.00251
AFIX 7
H2WA 2 0.639096 0.035381 0.591211 11.00000 -1.50000
H2WB 2 0.622368 0.137057 0.617633 11.00000 -1.50000
AFIX 0
O3 7 0.658590 0.272640 0.524683 11.00000 0.02227 0.03068 =
0.02763 0.00045 0.01319 -0.00264
O3W 7 0.500000 0.519698 0.250000 10.50000 0.07292 0.03462 =
0.03182 0.00000 0.02749 0.00000
AFIX 7
H3WA 2 0.482540 0.485948 0.212450 10.50000 -1.50000
H3WB 2 0.478570 0.485948 0.266590 10.50000 -1.50000
AFIX 0
O4 7 0.677873 0.386361 0.644338 11.00000 0.02384 0.02469 =
0.02581 0.00115 0.01013 0.00296
O4W 7 0.500000 0.947527 0.250000 10.50000 0.05122 0.03035 =
0.05026 0.00000 0.03311 0.00000
AFIX 7
H4WA 2 0.477934 0.979157 0.265195 10.50000 -1.50000
H4WB 2 0.483805 0.979157 0.212930 10.50000 -1.50000
AFIX 0
O5 7 0.620281 0.484746 0.705069 11.00000 0.04341 0.03168 =
0.02179 -0.00041 0.01712 0.00233
O6 7 0.519690 0.483333 0.587355 11.00000 0.02492 0.02311 =
0.01954 -0.00150 0.01329 -0.00188
AFIX 13
H6 2 0.503427 0.552540 0.603743 10.83333 -1.20000
AFIX 0
O7 7 0.619861 0.643173 0.614451 11.00000 0.02883 0.02376 =
0.01761 -0.00427 0.01156 -0.00192
O8 7 0.583787 0.471421 0.530556 11.00000 0.01975 0.01614 =
0.01754 -0.00151 0.00959 -0.00146
AFIX 13
H8 2 0.596869 0.401065 0.511514 10.83333 -1.20000
AFIX 0
O9 7 0.684298 0.631010 0.547374 11.00000 0.02262 0.04058 =
0.03063 -0.00717 0.01364 -0.00385
O10 7 0.625653 0.859527 0.547855 11.00000 0.04045 0.02203 =
0.03522 -0.00490 0.02187 -0.01023
O11 7 0.519999 0.694140 0.502448 11.00000 0.02232 0.01773 =
0.01908 -0.00130 0.01400 -0.00109
AFIX 13
H11 2 0.504255 0.758195 0.521512 10.83333 -1.20000
AFIX 0
O12 7 0.581939 0.673881 0.449965 11.00000 0.02082 0.02585 =
0.01890 -0.00011 0.01219 -0.00132
O13 7 0.511305 0.904147 0.420476 11.00000 0.04172 0.01920 =
0.03755 0.00086 0.01806 -0.00237
O14 7 0.422915 0.725521 0.384798 11.00000 0.02417 0.02299 =
0.02670 -0.00203 0.01489 -0.00083
O15 7 0.500256 0.719387 0.334195 11.00000 0.02587 0.03734 =
0.01908 0.00367 0.01337 -0.00025
N1 6 0.591948 0.740228 0.291851 11.00000 0.02275 0.03313 =
0.01898 0.00083 0.00879 0.00223
N2 6 0.712376 0.623752 0.433814 11.00000 0.03062 0.02611 =
0.02045 -0.00110 0.01178 0.00792
AFIX 43
H2 2 0.708964 0.662606 0.463201 11.00000 -1.20000
AFIX 0
N3 6 0.766907 0.349812 0.592925 11.00000 0.02375 0.02678 =
0.02328 -0.00114 0.01043 -0.00008
C1 1 0.621296 0.794044 0.263870 11.00000 0.02802 0.03721 =
0.01767 0.00270 0.00832 -0.00321
AFIX 43
H1 2 0.600460 0.836314 0.226449 11.00000 -1.20000
AFIX 0
C2 1 0.680074 0.789319 0.287916 11.00000 0.02608 0.04686 =
0.02785 0.00088 0.01450 -0.00724
AFIX 43
H2A 2 0.698529 0.825640 0.266561 11.00000 -1.20000
AFIX 0
C3 1 0.712292 0.730129 0.344372 11.00000 0.02064 0.04285 =
0.02871 -0.00463 0.00855 -0.00529
AFIX 43
H3 2 0.752437 0.724612 0.361381 11.00000 -1.20000
AFIX 0
C4 1 0.682856 0.679858 0.374356 11.00000 0.02471 0.02229 =
0.02047 -0.00103 0.00849 0.00466
C5 1 0.622881 0.685313 0.346505 11.00000 0.02264 0.03141 =
0.02236 0.00052 0.01165 0.00151
AFIX 43
H5 2 0.603423 0.649095 0.366847 11.00000 -1.20000
AFIX 0
C6 1 0.745499 0.511560 0.445370 11.00000 0.01711 0.02171 =
0.02475 0.00186 0.01136 -0.00326
C7 1 0.772102 0.465479 0.510245 11.00000 0.01987 0.02011 =
0.02449 -0.00384 0.00953 0.00135
C8 1 0.829323 0.503244 0.548968 11.00000 0.02395 0.02891 =
0.03166 -0.00020 0.01342 -0.00247
AFIX 43
H8A 2 0.850522 0.554568 0.534456 11.00000 -1.20000
AFIX 0
C9 1 0.853494 0.463303 0.608527 11.00000 0.01791 0.04604 =
0.02966 0.00122 0.00388 -0.00366
AFIX 43
H9 2 0.891557 0.486603 0.634813 11.00000 -1.20000
AFIX 0
C10 1 0.821545 0.389078 0.629277 11.00000 0.02832 0.03734 =
0.02238 0.00053 0.00625 -0.00178
AFIX 43
H10 2 0.838272 0.364840 0.670118 11.00000 -1.20000
AFIX 0
C11 1 0.742344 0.387529 0.534125 11.00000 0.01956 0.01916 =
0.01927 -0.00119 0.00891 0.00244
C12 1 0.680295 0.340375 0.496033 11.00000 0.01873 0.02140 =
0.02757 -0.00370 0.01212 0.00183
PART 2
O5W 7 0.467592 1.104417 0.322215 10.50000 0.13297 0.08237 =
0.10342 -0.02194 0.07210 -0.00318
PART 0
AFIX 6
O6W 7 0.350835 1.158849 0.298290 11.00000 0.15051 0.07231 =
0.05481 -0.02483 0.00232 0.04071
H6WA 2 0.352658 1.228487 0.319456 11.00000 -1.50000
H6WB 2 0.385605 1.130869 0.312802 11.00000 -1.50000
AFIX 6
O7W 7 0.260459 1.038679 0.262365 10.50000 0.09609 0.11899 =
0.09246 0.03796 0.02989 0.00024
H7WA 2 0.249196 1.030915 0.224396 10.50000 -1.50000
H7WB 2 0.295799 1.062156 0.276822 10.50000 -1.50000
AFIX 6
O8W 7 0.452797 0.842388 0.533867 11.00000 0.04373 0.03946 =
0.10570 -0.03767 0.03991 -0.01015
H8WA 2 0.457716 0.925197 0.544933 11.00000 -1.50000
H8WB 2 0.417037 0.822638 0.518788 11.00000 -1.50000
AFIX 0
O9W 7 0.466563 0.632010 0.641629 11.00000 0.06143 0.05361 =
0.04495 -0.00490 0.02852 0.00306
H9WA 2 0.431373 0.635721 0.619888 11.00000 0.11016
H9WB 2 0.491839 0.685312 0.663019 11.00000 0.11880
AFIX 6
O10W 7 0.618158 0.639430 0.800386 10.50000 0.16007 0.09492 =
0.16146 -0.05407 0.12279 -0.04677
H10A 2 0.603574 0.592709 0.818922 10.50000 -1.50000
H10B 2 0.609921 0.595234 0.767873 10.50000 -1.50000
AFIX 0
PART 1
O16 7 0.477604 1.117666 0.323213 10.50000 0.12967 0.07922 =
0.09701 -0.01386 0.07354 -0.01137
C13 1 0.445145 1.157943 0.276257 10.50000 0.16161 0.10385 =
0.06592 0.00787 0.02181 0.02578
HKLF 4
REM 111_a.res in C2/c
REM R1 = 0.0340 for 5127 Fo > 4sig(Fo) and 0.0551 for all 6756 data
REM 442 parameters refined using 13 restraints
END
WGHT 0.0287 0.6109
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1, -z+1
HTAB O1W O7W_$1
EQIV $2 x+1/2, -y+3/2, z+1/2
HTAB O1W O6W_$2
HTAB O1W O7W_$2
EQIV $3 x, y-1, z
HTAB O2W O10_$3
HTAB O2W O14_$1
EQIV $4 x, -y+1, z-1/2
HTAB O3W O9W_$4
HTAB O3W O9W_$1
HTAB O3W O10W_$1
HTAB O4W O5W
HTAB O4W O16
EQIV $5 -x+1, y, -z+1/2
HTAB O4W O5W_$5
HTAB O4W O16_$5
HTAB O6 O9W
HTAB O8 O3
HTAB O11 O8W
HTAB N2 O9
HTAB C1 O15_$5
HTAB C2 O7W_$5
EQIV $6 -x+3/2, -y+3/2, -z+1
HTAB C3 O9_$6
HTAB C5 O12
HTAB C5 O15
EQIV $7 -x+3/2, y-1/2, -z+3/2
HTAB C10 O10W_$7
EQIV $8 -x+1, -y+2, -z+1
HTAB O6W O7_$8
HTAB O6W O5W
HTAB O6W O16
EQIV $9 x-1/2, -y+3/2, z-1/2
HTAB O7W O4_$9
HTAB O7W O6W
HTAB O8W O13_$8
HTAB O8W O3_$1
HTAB O9W O2_$1
HTAB O9W O5W_$8
HTAB O9W O16_$8
EQIV $10 -x+1, y, -z+3/2
HTAB O10W O9W_$10
HTAB O10W O5
REM Highest difference peak 0.697, deepest hole -0.657, 1-sigma level 0.124
Q1 1 0.6129 0.4523 0.6715 11.00000 0.05 0.70
Q2 1 0.8006 0.1311 0.6903 11.00000 0.05 0.56
Q3 1 0.6218 0.6370 0.5816 11.00000 0.05 0.50
Q4 1 0.6146 0.6891 0.4989 11.00000 0.05 0.49
Q5 1 0.4873 0.7318 0.4599 11.00000 0.05 0.48
Q6 1 0.6568 0.7644 0.5164 11.00000 0.05 0.47
Q7 1 0.5931 0.7196 0.4894 11.00000 0.05 0.47
Q8 1 0.6144 0.7068 0.8293 11.00000 0.05 0.46
Q9 1 0.7470 0.2370 0.6528 11.00000 0.05 0.45
Q10 1 0.7751 0.5173 0.4334 11.00000 0.05 0.45
Q11 1 0.6468 0.2626 0.6205 11.00000 0.05 0.45
Q12 1 0.7377 0.5210 0.3986 11.00000 0.05 0.44
Q13 1 0.6480 0.7595 0.2821 11.00000 0.05 0.44
Q14 1 0.4676 0.6909 0.4487 11.00000 0.05 0.44
Q15 1 0.5476 0.4865 0.5004 11.00000 0.05 0.43
Q16 1 0.6729 0.6849 0.5553 11.00000 0.05 0.43
Q17 1 0.3231 1.0443 0.2906 11.00000 0.05 0.43
Q18 1 0.4874 0.6987 0.3568 11.00000 0.05 0.42
Q19 1 0.6090 0.6984 0.6082 11.00000 0.05 0.42
Q20 1 0.6119 0.4572 0.5623 11.00000 0.05 0.42
;
_shelx_res_checksum 29516
#######################################################################
#
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1540682'
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_audit_creation_date 2017-10-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'Cr H5 Mo6 O24, C31 H38 Cu3 N8 O12, C H2 O, 4(H2 O)'
_chemical_formula_sum 'C32 H53 Cr Cu3 Mo6 N8 O41'
_chemical_formula_weight 2024.08
_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'
Cr Cr 0.3209 0.6236 '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 9.624(2)
_cell_length_b 13.716(4)
_cell_length_c 14.061(3)
_cell_angle_alpha 61.168(4)
_cell_angle_beta 70.680(5)
_cell_angle_gamma 88.297(5)
_cell_volume 1515.4(6)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 3639
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 28.04
_cell_measurement_theta_min 2.27
_shelx_estimated_absorpt_T_max 0.770
_shelx_estimated_absorpt_T_min 0.705
_exptl_absorpt_coefficient_mu 2.508
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.5201
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0690 before and 0.0432 after correction. The Ratio of minimum to maximum transmission is 0.6975. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 2.218
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 992
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.11
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0307
_diffrn_reflns_av_unetI/netI 0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 8589
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full 25.050
_diffrn_reflns_theta_max 25.050
_diffrn_reflns_theta_min 1.716
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4327
_reflns_number_total 5309
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_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 'Bruker SHELXTL'
_refine_diff_density_max 2.354
_refine_diff_density_min -1.076
_refine_diff_density_rms 0.224
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.001
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 492
_refine_ls_number_reflns 5309
_refine_ls_number_restraints 98
_refine_ls_R_factor_all 0.0664
_refine_ls_R_factor_gt 0.0547
_refine_ls_restrained_S_all 0.999
_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^)+(0.1241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1550
_refine_ls_wR_factor_ref 0.1641
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
At 1.5 times of:
All C(H,H,H) groups, All C(H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
H17B-C17
0.93 with sigma of 0.02
H17A-C17
0.93 with sigma of 0.02
H5WA-H8
2.13 with sigma of 0.02
C14-N4 \\sim N4-C15 \\sim C15A-N14 \\sim N14-C14A
with sigma of 0.02
C13-O1F \\sim O1F-C13A
with sigma of 0.02
H16B-O1A \\sim H17A-O2A
with sigma of 0.02
H17B-O2A \\sim H16A-O1A
with sigma of 0.02
H17A-H17B \\sim H16A-H16B
with sigma of 0.02
3. Rigid bond restraints
O1A, O2W, C16, C17, O2A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C14A \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C16 \\sim O1A \\sim C17 \\sim O2A \\sim O2W: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O2W \\sim O1A \\sim C16 \\sim O2A \\sim C17: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
N4, C13, H13, N14, C15, H15A, H15B, C14, H14A, H14B, H14C, C14A, H14D, H14E,
H14F, C13A, H13A, C15A, H15D, H15E
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(N14)=Sof(C13A)=Sof(H13A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
Sof(N4)=Sof(C13)=Sof(H13)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
Fixed Sof: H5(0.83333) H7(0.83333) H8(0.83333) O1A(0.5) O2W(0.5) H2WA(0.5)
H2WB(0.5) C16(0.5) H16A(0.5) H16B(0.5) O2A(0.5) C17(0.5) H17A(0.5) H17B(0.5)
7.a Free rotating group:
O4W(H4WA,H4WB), O5W(H5WA,H5WB)
7.b Rotating group:
O1W(H1WA,H1WB), O2W(H2WA,H2WB)
7.c Ternary CH refined with riding coordinates:
O5(H5), O7(H7), O8(H8)
7.d Aromatic/amide H refined with riding coordinates:
N2(H2), C3(H3), C2(H2A), C1(H1), C12(H12), C11(H11), C10(H10), C9(H9),
C13(H13), C13A(H13A)
7.e X=CH2 refined with riding coordinates:
C16(H16A,H16B)
7.f Idealised Me refined as rotating group:
C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15A(H15D,
H15E,H15F)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.52045(6) 0.25363(5) 1.00746(5) 0.02861(19) Uani 1 1 d . . . . .
Mo2 Mo 0.37196(6) 0.45127(4) 0.83218(4) 0.02636(19) Uani 1 1 d . . . . .
Mo3 Mo 0.35175(6) 0.69753(5) 0.82075(5) 0.02735(19) Uani 1 1 d . . . . .
Cr1 Cr 0.5000 0.5000 1.0000 0.0208(3) Uani 1 2 d S T P . .
O1 O 0.6302(6) 0.2381(4) 0.8938(5) 0.0431(12) Uani 1 1 d . . . . .
O2 O 0.4328(6) 0.1228(4) 1.1188(4) 0.0436(12) Uani 1 1 d . . . . .
O3 O 0.3526(5) 0.3064(4) 0.9631(4) 0.0318(10) Uani 1 1 d . . . . .
O4 O 0.4767(6) 0.4347(4) 0.7176(4) 0.0401(12) Uani 1 1 d . . . . .
O5 O 0.5754(5) 0.4468(4) 0.8882(4) 0.0269(9) Uani 1 1 d . . . . .
H5 H 0.6749 0.4803 0.8279 0.032 Uiso 0.8333 1 calc R . . . .
O16 O 0.1925(5) 0.4457(4) 0.8368(4) 0.0405(11) Uani 1 1 d . . . . .
O7 O 0.3198(4) 0.5112(3) 0.9622(3) 0.0241(9) Uani 1 1 d . . . . .
H7 H 0.2237 0.4793 1.0271 0.029 Uiso 0.8333 1 calc R . . . .
O8 O 0.5533(5) 0.6632(4) 0.8805(4) 0.0269(9) Uani 1 1 d . . . . .
H8 H 0.6535 0.6900 0.8205 0.032 Uiso 0.8333 1 calc DR . . . .
O9 O 0.4357(5) 0.6131(4) 0.7473(4) 0.0314(10) Uani 1 1 d . . . . .
O10 O 0.4319(6) 0.8290(4) 0.7031(4) 0.0393(11) Uani 1 1 d . . . . .
O11 O 0.3146(5) 0.7230(4) 0.9500(4) 0.0320(10) Uani 1 1 d . . . . .
O12 O 0.1711(5) 0.6845(4) 0.8317(5) 0.0430(12) Uani 1 1 d . . . . .
Cu1 Cu 0.90028(10) 0.30619(7) 0.77156(7) 0.0368(2) Uani 1 1 d . . . . .
Cu2 Cu 0.5000 1.0000 0.5000 0.0360(3) Uani 1 2 d S T P . .
O1W O 0.9474(5) 0.2923(4) 0.9025(4) 0.0396(11) Uani 1 1 d . . . . .
H1WA H 1.0231 0.3434 0.8782 0.059 Uiso 1 1 d GR . . . .
H1WB H 0.8961 0.2614 0.9825 0.059 Uiso 1 1 d GR . . . .
O1A O 0.724(5) 0.984(4) 0.493(5) 0.040(4) Uani 0.5 1 d D U . A 2
O1F O 0.9033(7) 0.1471(5) 0.8218(6) 0.0559(14) Uani 1 1 d D . . . .
O2W O 0.706(5) 0.988(4) 0.488(5) 0.042(5) Uani 0.5 1 d . U . A 3
H2WA H 0.7154 0.9201 0.5331 0.063 Uiso 0.5 1 d GR . . A 3
H2WB H 0.7339 1.0268 0.5138 0.063 Uiso 0.5 1 d GR . . A 3
O13 O 0.8664(6) 0.4606(4) 0.7283(4) 0.0380(11) Uani 1 1 d . . . . .
O14 O 0.8189(6) 0.6134(5) 0.5911(5) 0.0467(13) Uani 1 1 d . . . . .
O15 O 0.8307(6) 0.6685(4) 0.3207(4) 0.0416(12) Uani 1 1 d . . . . .
N1 N 0.8534(6) 0.3413(5) 0.6329(5) 0.0338(12) Uani 1 1 d . . . . .
N2 N 0.6187(6) 0.6253(5) 0.4729(5) 0.0311(12) Uani 1 1 d . . . . .
H2 H 0.5607 0.5727 0.5399 0.037 Uiso 1 1 calc R . . . .
N3 N 0.5124(6) 0.8976(5) 0.4327(5) 0.0328(12) Uani 1 1 d . . . . .
N4 N 1.0008(11) -0.0111(9) 0.8608(11) 0.067(3) Uani 0.742(13) 1 d D U . B 1
C6 C 0.8193(7) 0.4454(6) 0.5807(6) 0.0327(14) Uani 1 1 d . . . . .
C4 C 0.7806(7) 0.4867(5) 0.4830(6) 0.0305(14) Uani 1 1 d . . . . .
C3 C 0.7833(8) 0.4156(6) 0.4365(6) 0.0395(16) Uani 1 1 d . . . . .
H3 H 0.7621 0.4403 0.3692 0.047 Uiso 1 1 calc R . . . .
C2 C 0.8178(9) 0.3090(7) 0.4917(7) 0.0444(18) Uani 1 1 d . . . . .
H2A H 0.8176 0.2607 0.4628 0.053 Uiso 1 1 calc R . . . .
C1 C 0.8518(8) 0.2744(6) 0.5878(6) 0.0368(16) Uani 1 1 d . . . . .
H1 H 0.8749 0.2021 0.6240 0.044 Uiso 1 1 calc R . . . .
C7 C 0.8345(7) 0.5151(6) 0.6348(6) 0.0315(14) Uani 1 1 d . . . . .
C5 C 0.7460(7) 0.6035(6) 0.4190(5) 0.0306(14) Uani 1 1 d . . . . .
C8 C 0.5748(7) 0.7347(5) 0.4225(6) 0.0321(14) Uani 1 1 d . . . . .
C12 C 0.5575(7) 0.7973(6) 0.4754(6) 0.0326(14) Uani 1 1 d . . . . .
H12 H 0.5777 0.7695 0.5434 0.039 Uiso 1 1 calc R . . . .
C11 C 0.4808(9) 0.9354(6) 0.3348(6) 0.0403(17) Uani 1 1 d . . . . .
H11 H 0.4435 1.0031 0.3071 0.048 Uiso 1 1 calc R . . . .
C10 C 0.5010(10) 0.8792(6) 0.2756(6) 0.0469(19) Uani 1 1 d . . . . .
H10 H 0.4826 0.9097 0.2066 0.056 Uiso 1 1 calc R . . . .
C9 C 0.5496(9) 0.7750(6) 0.3190(6) 0.0427(18) Uani 1 1 d . . . . .
H9 H 0.5646 0.7342 0.2804 0.051 Uiso 1 1 calc R . . . .
C13 C 1.0027(15) 0.0977(10) 0.8141(12) 0.067(4) Uani 0.742(13) 1 d D U . B 1
H13 H 1.0964 0.1416 0.7683 0.081 Uiso 0.742(13) 1 calc R U . B 1
N14 N 0.867(5) -0.026(3) 0.937(2) 0.076(11) Uani 0.258(13) 1 d D U . B 2
C15 C 1.132(2) -0.0590(17) 0.832(2) 0.169(14) Uani 0.742(13) 1 d D U . B 1
H15A H 1.1075 -0.1186 0.8205 0.253 Uiso 0.742(13) 1 calc GR U . B 1
H15B H 1.1683 -0.0886 0.8953 0.253 Uiso 0.742(13) 1 calc GR U . B 1
H15C H 1.2067 -0.0019 0.7627 0.253 Uiso 0.742(13) 1 calc GR . . B 1
C16 C 0.799(2) 1.0651(19) 0.4330(19) 0.069(4) Uani 0.5 1 d . U . A 2
H16A H 0.7609 1.1293 0.3927 0.083 Uiso 0.5 1 calc DR . . A 2
H16B H 0.8993 1.0694 0.4222 0.083 Uiso 0.5 1 calc DR . . A 2
O2A O 0.9390(16) 1.0815(15) 0.4287(15) 0.096(4) Uani 0.5 1 d D U . C -1
C17 C 0.928(2) 1.1609(19) 0.3476(19) 0.071(4) Uani 0.5 1 d D U . C -1
O4W O 0.0822(6) 0.4268(6) 1.1549(5) 0.0601(17) Uani 1 1 d . . . . .
H4WA H 0.0657 0.4242 1.2195 0.090 Uiso 1 1 d G . . . .
H4WB H 0.0349 0.3683 1.1669 0.090 Uiso 1 1 d G . . . .
O5W O 0.7863(7) 0.7776(6) 0.6618(6) 0.0673(18) Uani 1 1 d . . . . .
H5WA H 0.8661 0.7556 0.6865 0.101 Uiso 1 1 d DG . . . .
H5WB H 0.7647 0.7221 0.6497 0.101 Uiso 1 1 d G . . . .
C14 C 0.866(2) -0.078(2) 0.958(2) 0.082(9) Uani 0.49(3) 1 d D U . B 1
H14A H 0.8865 -0.1129 1.0288 0.123 Uiso 0.49(3) 1 calc GR U . B 1
H14B H 0.8296 -0.1351 0.9475 0.123 Uiso 0.49(3) 1 calc GR U . B 1
H14C H 0.7918 -0.0303 0.9628 0.123 Uiso 0.49(3) 1 calc GR U . B 1
C14A C 0.921(5) -0.071(2) 0.861(3) 0.142(15) Uani 0.51(3) 1 d D U . B 2
H14D H 0.8614 -0.0544 0.8137 0.213 Uiso 0.51(3) 1 calc GR U . B 2
H14E H 0.9155 -0.1510 0.9060 0.213 Uiso 0.51(3) 1 calc GR U . B 2
H14F H 1.0229 -0.0371 0.8116 0.213 Uiso 0.51(3) 1 calc GR U . B 2
C13A C 0.857(3) 0.066(2) 0.909(2) 0.056(9) Uani 0.258(13) 1 d D U . B 2
H13A H 0.7992 0.0768 0.9701 0.067 Uiso 0.258(13) 1 calc R U . B 2
C15A C 0.800(4) -0.115(3) 1.054(2) 0.078(11) Uani 0.258(13) 1 d D U . B 2
H15D H 0.6937 -0.1237 1.0760 0.117 Uiso 0.258(13) 1 calc GR U . B 2
H15E H 0.8277 -0.0975 1.1044 0.117 Uiso 0.258(13) 1 calc GR U . B 2
H15F H 0.8338 -0.1838 1.0607 0.117 Uiso 0.258(13) 1 calc GR . . B 2
H17A H 0.987(7) 1.168(7) 0.278(4) 0.117 Uiso 0.5 1 d DR . . D -1
H17B H 0.838(11) 1.185(14) 0.360(6) 0.117 Uiso 0.5 1 d DR . . E -1
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
Mo1 0.0349(4) 0.0267(3) 0.0293(3) -0.0143(3) -0.0172(3) 0.0077(2)
Mo2 0.0316(3) 0.0284(3) 0.0244(3) -0.0137(2) -0.0155(3) 0.0049(2)
Mo3 0.0311(3) 0.0275(3) 0.0276(3) -0.0131(3) -0.0167(3) 0.0074(2)
Cr1 0.0228(7) 0.0228(7) 0.0197(6) -0.0109(6) -0.0108(6) 0.0049(5)
O1 0.047(3) 0.041(3) 0.049(3) -0.028(3) -0.018(3) 0.012(2)
O2 0.056(3) 0.032(3) 0.044(3) -0.014(2) -0.028(3) 0.007(2)
O3 0.032(2) 0.034(3) 0.031(2) -0.013(2) -0.017(2) 0.0016(19)
O4 0.054(3) 0.039(3) 0.031(2) -0.020(2) -0.014(2) 0.003(2)
O5 0.028(2) 0.031(2) 0.023(2) -0.0149(19) -0.0087(19) 0.0047(18)
O16 0.042(3) 0.044(3) 0.045(3) -0.021(2) -0.029(2) 0.005(2)
O7 0.023(2) 0.029(2) 0.022(2) -0.0121(18) -0.0111(18) 0.0038(17)
O8 0.028(2) 0.029(2) 0.025(2) -0.0125(19) -0.0122(19) 0.0057(18)
O9 0.035(3) 0.033(3) 0.029(2) -0.016(2) -0.016(2) 0.0083(19)
O10 0.052(3) 0.034(3) 0.036(3) -0.017(2) -0.022(2) 0.008(2)
O11 0.033(2) 0.038(3) 0.036(2) -0.021(2) -0.020(2) 0.012(2)
O12 0.037(3) 0.047(3) 0.057(3) -0.027(3) -0.030(3) 0.013(2)
Cu1 0.0462(5) 0.0369(5) 0.0332(5) -0.0174(4) -0.0220(4) 0.0146(4)
Cu2 0.0388(7) 0.0400(7) 0.0435(7) -0.0284(6) -0.0200(6) 0.0140(5)
O1W 0.034(3) 0.052(3) 0.030(2) -0.018(2) -0.013(2) 0.007(2)
O1A 0.044(8) 0.044(5) 0.048(6) -0.025(5) -0.034(6) 0.028(6)
O1F 0.062(4) 0.044(3) 0.071(4) -0.028(3) -0.039(3) 0.022(3)
O2W 0.048(9) 0.046(6) 0.050(6) -0.028(5) -0.032(7) 0.021(7)
O13 0.052(3) 0.037(3) 0.034(2) -0.019(2) -0.025(2) 0.011(2)
O14 0.057(3) 0.045(3) 0.050(3) -0.027(3) -0.030(3) 0.019(3)
O15 0.041(3) 0.038(3) 0.032(3) -0.010(2) -0.009(2) 0.011(2)
N1 0.039(3) 0.030(3) 0.036(3) -0.016(3) -0.019(3) 0.013(2)
N2 0.033(3) 0.031(3) 0.026(3) -0.011(2) -0.011(2) 0.008(2)
N3 0.039(3) 0.029(3) 0.035(3) -0.017(2) -0.018(3) 0.009(2)
N4 0.066(6) 0.038(5) 0.094(8) -0.024(5) -0.038(6) 0.016(4)
C6 0.028(3) 0.036(4) 0.030(3) -0.016(3) -0.006(3) 0.002(3)
C4 0.025(3) 0.030(3) 0.031(3) -0.012(3) -0.008(3) 0.005(3)
C3 0.043(4) 0.044(4) 0.040(4) -0.024(3) -0.022(3) 0.014(3)
C2 0.050(5) 0.045(4) 0.052(4) -0.033(4) -0.020(4) 0.012(3)
C1 0.042(4) 0.044(4) 0.039(4) -0.026(3) -0.025(3) 0.017(3)
C7 0.027(3) 0.036(4) 0.035(3) -0.020(3) -0.012(3) 0.006(3)
C5 0.032(4) 0.039(4) 0.025(3) -0.017(3) -0.014(3) 0.009(3)
C8 0.033(4) 0.028(3) 0.031(3) -0.012(3) -0.012(3) 0.009(3)
C12 0.038(4) 0.037(4) 0.031(3) -0.020(3) -0.019(3) 0.011(3)
C11 0.059(5) 0.036(4) 0.039(4) -0.019(3) -0.032(4) 0.019(3)
C10 0.079(6) 0.043(4) 0.037(4) -0.024(4) -0.038(4) 0.028(4)
C9 0.063(5) 0.040(4) 0.041(4) -0.026(4) -0.030(4) 0.020(4)
C13 0.053(7) 0.041(5) 0.076(8) -0.011(5) -0.015(6) 0.012(5)
N14 0.10(3) 0.055(13) 0.095(16) -0.043(12) -0.063(15) 0.045(13)
C15 0.112(11) 0.067(11) 0.20(2) -0.017(12) 0.003(13) 0.046(9)
C16 0.056(6) 0.069(6) 0.073(6) -0.023(5) -0.033(5) 0.018(5)
O2A 0.061(6) 0.093(8) 0.103(7) -0.021(6) -0.037(6) 0.006(6)
C17 0.054(7) 0.070(8) 0.084(8) -0.026(6) -0.038(6) 0.015(6)
O4W 0.037(3) 0.088(5) 0.061(4) -0.048(4) -0.007(3) -0.010(3)
O5W 0.061(4) 0.078(5) 0.087(5) -0.060(4) -0.027(4) 0.012(3)
C14 0.070(9) 0.051(11) 0.094(12) -0.006(9) -0.042(8) 0.013(8)
C14A 0.25(4) 0.060(14) 0.101(16) -0.047(13) -0.045(18) 0.044(18)
C13A 0.08(2) 0.052(13) 0.076(17) -0.039(13) -0.064(17) 0.041(13)
C15A 0.11(3) 0.056(15) 0.094(15) -0.043(12) -0.064(16) 0.035(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.706(5) . ?
Mo1 O2 1.699(5) . ?
Mo1 O3 1.919(4) . ?
Mo1 O5 2.307(4) . ?
Mo1 O8 2.287(4) 2_667 ?
Mo1 O11 1.955(4) 2_667 ?
Mo2 O3 1.908(4) . ?
Mo2 O4 1.712(5) . ?
Mo2 O5 2.329(4) . ?
Mo2 O16 1.710(5) . ?
Mo2 O7 2.256(4) . ?
Mo2 O9 1.942(5) . ?
Mo3 O7 2.306(4) . ?
Mo3 O8 2.309(4) . ?
Mo3 O9 1.899(4) . ?
Mo3 O10 1.716(5) . ?
Mo3 O11 1.931(4) . ?
Mo3 O12 1.701(5) . ?
Cr1 O5 1.962(4) . ?
Cr1 O5 1.962(4) 2_667 ?
Cr1 O7 1.957(4) 2_667 ?
Cr1 O7 1.957(4) . ?
Cr1 O8 1.992(4) 2_667 ?
Cr1 O8 1.992(4) . ?
O8 Mo1 2.287(4) 2_667 ?
O11 Mo1 1.955(4) 2_667 ?
Cu1 O1W 1.961(5) . ?
Cu1 O1F 1.945(6) . ?
Cu1 O13 1.951(5) . ?
Cu1 O15 2.429(5) 2_766 ?
Cu1 N1 1.975(6) . ?
Cu2 O1A 2.14(4) 2_676 ?
Cu2 O1A 2.14(4) . ?
Cu2 O2W 1.94(4) . ?
Cu2 O2W 1.94(4) 2_676 ?
Cu2 N3 2.020(5) 2_676 ?
Cu2 N3 2.020(5) . ?
O1A C16 1.10(5) . ?
O1F C13 1.162(12) . ?
O1F C13A 1.14(2) . ?
O13 C7 1.298(8) . ?
O14 C7 1.211(8) . ?
O15 Cu1 2.429(5) 2_766 ?
O15 C5 1.216(8) . ?
N1 C6 1.344(9) . ?
N1 C1 1.347(8) . ?
N2 C5 1.321(8) . ?
N2 C8 1.438(8) . ?
N3 C12 1.335(8) . ?
N3 C11 1.355(8) . ?
N4 C13 1.306(15) . ?
N4 C15 1.430(16) . ?
N4 C14 1.444(17) . ?
C6 C4 1.386(9) . ?
C6 C7 1.517(9) . ?
C4 C3 1.408(9) . ?
C4 C5 1.505(9) . ?
C3 C2 1.378(10) . ?
C2 C1 1.351(10) . ?
C8 C12 1.358(9) . ?
C8 C9 1.390(9) . ?
C11 C10 1.353(10) . ?
C10 C9 1.393(10) . ?
N14 C14A 1.428(19) . ?
N14 C13A 1.14(4) . ?
N14 C15A 1.42(2) . ?
O2A C17 1.17(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O3 102.1(2) . . ?
O1 Mo1 O5 89.7(2) . . ?
O1 Mo1 O8 156.7(2) . 2_667 ?
O1 Mo1 O11 94.9(2) . 2_667 ?
O2 Mo1 O1 107.0(2) . . ?
O2 Mo1 O3 97.4(2) . . ?
O2 Mo1 O5 161.8(2) . . ?
O2 Mo1 O8 94.1(2) . 2_667 ?
O2 Mo1 O11 102.0(2) . 2_667 ?
O3 Mo1 O5 71.59(17) . . ?
O3 Mo1 O8 84.36(17) . 2_667 ?
O3 Mo1 O11 149.13(19) . 2_667 ?
O8 Mo1 O5 70.88(15) 2_667 . ?
O11 Mo1 O5 83.07(17) 2_667 . ?
O11 Mo1 O8 70.58(16) 2_667 2_667 ?
O3 Mo2 O5 71.26(17) . . ?
O3 Mo2 O7 84.54(17) . . ?
O3 Mo2 O9 150.05(18) . . ?
O4 Mo2 O3 102.5(2) . . ?
O4 Mo2 O5 91.7(2) . . ?
O4 Mo2 O7 157.7(2) . . ?
O4 Mo2 O9 93.8(2) . . ?
O16 Mo2 O3 98.7(2) . . ?
O16 Mo2 O4 106.4(2) . . ?
O16 Mo2 O5 161.08(19) . . ?
O16 Mo2 O7 93.21(19) . . ?
O16 Mo2 O9 100.6(2) . . ?
O7 Mo2 O5 70.34(15) . . ?
O9 Mo2 O5 83.42(17) . . ?
O9 Mo2 O7 71.77(16) . . ?
O7 Mo3 O8 69.82(15) . . ?
O9 Mo3 O7 71.30(16) . . ?
O9 Mo3 O8 83.55(17) . . ?
O9 Mo3 O11 148.64(19) . . ?
O10 Mo3 O7 162.1(2) . . ?
O10 Mo3 O8 95.6(2) . . ?
O10 Mo3 O9 97.4(2) . . ?
O10 Mo3 O11 102.2(2) . . ?
O11 Mo3 O7 83.16(17) . . ?
O11 Mo3 O8 70.45(16) . . ?
O12 Mo3 O7 91.3(2) . . ?
O12 Mo3 O8 157.8(2) . . ?
O12 Mo3 O9 101.8(2) . . ?
O12 Mo3 O10 104.9(2) . . ?
O12 Mo3 O11 96.5(2) . . ?
O5 Cr1 O5 180.0 . 2_667 ?
O5 Cr1 O8 84.72(17) 2_667 . ?
O5 Cr1 O8 95.28(18) . . ?
O5 Cr1 O8 84.72(17) . 2_667 ?
O5 Cr1 O8 95.29(18) 2_667 2_667 ?
O7 Cr1 O5 95.25(17) . 2_667 ?
O7 Cr1 O5 95.24(17) 2_667 . ?
O7 Cr1 O5 84.75(17) . . ?
O7 Cr1 O5 84.75(17) 2_667 2_667 ?
O7 Cr1 O7 180.0 2_667 . ?
O7 Cr1 O8 83.96(18) 2_667 2_667 ?
O7 Cr1 O8 83.96(18) . . ?
O7 Cr1 O8 96.04(18) 2_667 . ?
O7 Cr1 O8 96.04(18) . 2_667 ?
O8 Cr1 O8 180.0 . 2_667 ?
Mo2 O3 Mo1 121.3(2) . . ?
Mo1 O5 Mo2 92.00(15) . . ?
Cr1 O5 Mo1 102.31(18) . . ?
Cr1 O5 Mo2 101.08(17) . . ?
Mo2 O7 Mo3 92.88(14) . . ?
Cr1 O7 Mo2 103.82(17) . . ?
Cr1 O7 Mo3 103.73(18) . . ?
Mo1 O8 Mo3 94.40(15) 2_667 . ?
Cr1 O8 Mo1 102.06(17) . 2_667 ?
Cr1 O8 Mo3 102.50(18) . . ?
Mo3 O9 Mo2 118.8(2) . . ?
Mo3 O11 Mo1 120.4(2) . 2_667 ?
O1W Cu1 O15 83.75(19) . 2_766 ?
O1W Cu1 N1 172.5(2) . . ?
O1F Cu1 O1W 92.7(2) . . ?
O1F Cu1 O13 171.8(2) . . ?
O1F Cu1 O15 86.3(2) . 2_766 ?
O1F Cu1 N1 94.8(2) . . ?
O13 Cu1 O1W 89.9(2) . . ?
O13 Cu1 O15 101.79(19) . 2_766 ?
O13 Cu1 N1 82.7(2) . . ?
N1 Cu1 O15 96.5(2) . 2_766 ?
O1A Cu2 O1A 180(3) . 2_676 ?
O2W Cu2 O2W 180.0 . 2_676 ?
O2W Cu2 N3 88(2) . . ?
O2W Cu2 N3 92(2) 2_676 . ?
O2W Cu2 N3 88(2) 2_676 2_676 ?
O2W Cu2 N3 92(2) . 2_676 ?
N3 Cu2 O1A 91(2) 2_676 . ?
N3 Cu2 O1A 89(2) . . ?
N3 Cu2 O1A 91(2) . 2_676 ?
N3 Cu2 O1A 89(2) 2_676 2_676 ?
N3 Cu2 N3 180.0 . 2_676 ?
C16 O1A Cu2 112(3) . . ?
C13 O1F Cu1 130.7(8) . . ?
C13A O1F Cu1 134.3(17) . . ?
C7 O13 Cu1 115.7(4) . . ?
C5 O15 Cu1 131.8(4) . 2_766 ?
C6 N1 Cu1 113.4(4) . . ?
C6 N1 C1 118.8(6) . . ?
C1 N1 Cu1 127.8(5) . . ?
C5 N2 C8 121.7(5) . . ?
C12 N3 Cu2 123.8(4) . . ?
C12 N3 C11 118.0(5) . . ?
C11 N3 Cu2 118.1(4) . . ?
C13 N4 C15 122.2(13) . . ?
C13 N4 C14 114.5(15) . . ?
C15 N4 C14 122.3(16) . . ?
N1 C6 C4 122.9(6) . . ?
N1 C6 C7 113.8(6) . . ?
C4 C6 C7 123.3(6) . . ?
C6 C4 C3 117.0(6) . . ?
C6 C4 C5 125.1(6) . . ?
C3 C4 C5 117.8(6) . . ?
C2 C3 C4 119.2(7) . . ?
C1 C2 C3 120.2(7) . . ?
N1 C1 C2 121.9(7) . . ?
O13 C7 C6 114.2(6) . . ?
O14 C7 O13 124.9(6) . . ?
O14 C7 C6 120.9(6) . . ?
O15 C5 N2 124.7(6) . . ?
O15 C5 C4 118.9(6) . . ?
N2 C5 C4 116.2(6) . . ?
C12 C8 N2 120.6(6) . . ?
C12 C8 C9 120.6(6) . . ?
C9 C8 N2 118.8(6) . . ?
N3 C12 C8 122.0(6) . . ?
C10 C11 N3 122.9(6) . . ?
C11 C10 C9 119.3(6) . . ?
C8 C9 C10 117.1(6) . . ?
O1F C13 N4 128.9(13) . . ?
C13A N14 C14A 126(3) . . ?
C13A N14 C15A 123(3) . . ?
C15A N14 C14A 110(3) . . ?
N14 C13A O1F 133(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Mo3 O9 Mo2 20.3(2) . . . . ?
O8 Mo3 O9 Mo2 91.2(2) . . . . ?
O10 Mo3 O9 Mo2 -174.0(3) . . . . ?
O11 Mo3 O9 Mo2 57.5(5) . . . . ?
O12 Mo3 O9 Mo2 -67.0(3) . . . . ?
Cu1 O1F C13 N4 171.1(12) . . . . ?
Cu1 O1F C13A N14 -175(4) . . . . ?
Cu1 O13 C7 O14 -175.4(5) . . . . ?
Cu1 O13 C7 C6 4.0(7) . . . . ?
Cu1 O15 C5 N2 150.2(5) 2_766 . . . ?
Cu1 O15 C5 C4 -34.0(9) 2_766 . . . ?
Cu1 N1 C6 C4 -179.0(5) . . . . ?
Cu1 N1 C6 C7 3.9(7) . . . . ?
Cu1 N1 C1 C2 -179.9(6) . . . . ?
Cu2 N3 C12 C8 -175.0(5) . . . . ?
Cu2 N3 C11 C10 172.7(7) . . . . ?
N1 C6 C4 C3 -2.2(10) . . . . ?
N1 C6 C4 C5 -178.0(6) . . . . ?
N1 C6 C7 O13 -5.3(9) . . . . ?
N1 C6 C7 O14 174.1(6) . . . . ?
N2 C8 C12 N3 -177.9(6) . . . . ?
N2 C8 C9 C10 177.3(7) . . . . ?
N3 C11 C10 C9 3.2(13) . . . . ?
C6 N1 C1 C2 0.4(11) . . . . ?
C6 C4 C3 C2 2.5(10) . . . . ?
C6 C4 C5 O15 112.7(7) . . . . ?
C6 C4 C5 N2 -71.1(8) . . . . ?
C4 C6 C7 O13 177.7(6) . . . . ?
C4 C6 C7 O14 -3.0(10) . . . . ?
C4 C3 C2 C1 -1.5(11) . . . . ?
C3 C4 C5 O15 -63.1(9) . . . . ?
C3 C4 C5 N2 113.1(7) . . . . ?
C3 C2 C1 N1 0.0(12) . . . . ?
C1 N1 C6 C4 0.8(10) . . . . ?
C1 N1 C6 C7 -176.3(6) . . . . ?
C7 C6 C4 C3 174.6(6) . . . . ?
C7 C6 C4 C5 -1.2(10) . . . . ?
C5 N2 C8 C12 -116.7(7) . . . . ?
C5 N2 C8 C9 63.7(9) . . . . ?
C5 C4 C3 C2 178.6(6) . . . . ?
C8 N2 C5 O15 -5.9(10) . . . . ?
C8 N2 C5 C4 178.1(6) . . . . ?
C12 N3 C11 C10 -3.8(12) . . . . ?
C12 C8 C9 C10 -2.4(11) . . . . ?
C11 N3 C12 C8 1.3(10) . . . . ?
C11 C10 C9 C8 0.0(12) . . . . ?
C9 C8 C12 N3 1.8(11) . . . . ?
C15 N4 C13 O1F 173(2) . . . . ?
C14 N4 C13 O1F -19(3) . . . . ?
C14A N14 C13A O1F -14(8) . . . . ?
C15A N14 C13A O1F 179(4) . . . . ?
_iucr_refine_instructions_details
;
20160913_sg01_0m.res created by SHELXL-2014/7
TITL 20160913_sg01_0m_a.res in P-1
rem EADP C15 C14A
rem EADP N14 C14
CELL 0.71073 9.6244 13.7158 14.0613 61.168 70.68 88.297
ZERR 1 0.0024 0.0036 0.0034 0.004 0.005 0.005
LATT 1
SFAC C H Cr Cu Mo N O
UNIT 32 53 1 3 6 8 41
EQIV $1 2-X,2-Y,1-Z
DFIX 0.93 H17b C17
DFIX 0.93 H17a C17
DFIX 2.13 H5Wa H8
SADI C14 N4 N4 C15 C15A N14 N14 C14A
SADI C13 O1F O1F C13A
SADI H16b O1A H17a O2A
SADI H17b O2A H16a O1A
SADI H17a H17b H16a H16b
DELU O1A O2W C16 C17 O2A
SIMU C14A C14
SIMU C16 O1A C17 O2A O2W
SIMU 0.01 0.01 2 O2W O1A C16 O2A C17
RIGU N4 C13 H13 N14 C15 H15a H15b C14 H14a H14b H14c C14A H14d H14e H14f =
C13A H13A C15A H15D H15E
L.S. 50
PLAN 50
SIZE 0.11 0.13 0.15
TEMP 23
FREE O2A O2A_$1
bump
conf
htab
bump
fmap 2
acta
OMIT 0 50.1
OMIT -4 7 12
OMIT -7 7 10
OMIT -7 6 9
OMIT -4 7 13
OMIT -6 7 9
OMIT -3 8 13
OMIT -6 6 9
OMIT -11 2 1
OMIT -9 2 5
OMIT -1 2 0
OMIT -1 8 17
OMIT -8 3 6
OMIT -9 4 4
OMIT -7 6 8
OMIT -1 1 0
OMIT 1 -2 2
OMIT -11 2 2
OMIT -7 7 8
OMIT -6 7 10
OMIT -9 3 6
OMIT 2 1 3
OMIT 2 2 3
OMIT 2 -3 2
OMIT -1 2 1
OMIT -2 -2 2
OMIT 1 3 0
OMIT 2 5 4
OMIT 2 -4 1
REM
REM
REM
WGHT 0.124100
FVAR 0.32241 0.74193 0.49204
MO1 5 0.520452 0.253628 1.007460 11.00000 0.03493 0.02671 =
0.02928 -0.01435 -0.01719 0.00772
MO2 5 0.371958 0.451272 0.832183 11.00000 0.03161 0.02843 =
0.02436 -0.01369 -0.01552 0.00491
MO3 5 0.351748 0.697531 0.820748 11.00000 0.03107 0.02750 =
0.02761 -0.01307 -0.01674 0.00735
CR1 3 0.500000 0.500000 1.000000 10.50000 0.02282 0.02280 =
0.01970 -0.01090 -0.01075 0.00485
O1 7 0.630153 0.238142 0.893812 11.00000 0.04653 0.04099 =
0.04917 -0.02818 -0.01756 0.01238
O2 7 0.432756 0.122848 1.118777 11.00000 0.05603 0.03155 =
0.04430 -0.01365 -0.02779 0.00703
O3 7 0.352627 0.306394 0.963113 11.00000 0.03207 0.03364 =
0.03092 -0.01349 -0.01657 0.00164
O4 7 0.476734 0.434655 0.717593 11.00000 0.05362 0.03907 =
0.03092 -0.02024 -0.01437 0.00322
O5 7 0.575353 0.446805 0.888243 11.00000 0.02777 0.03093 =
0.02339 -0.01489 -0.00872 0.00470
AFIX 13
H5 2 0.674865 0.480307 0.827943 10.83333 -1.20000
AFIX 0
O16 7 0.192463 0.445717 0.836757 11.00000 0.04235 0.04406 =
0.04511 -0.02118 -0.02911 0.00477
O7 7 0.319775 0.511228 0.962177 11.00000 0.02329 0.02882 =
0.02192 -0.01212 -0.01113 0.00384
AFIX 13
H7 2 0.223692 0.479333 1.027120 10.83333 -1.20000
AFIX 0
O8 7 0.553277 0.663227 0.880533 11.00000 0.02774 0.02878 =
0.02510 -0.01249 -0.01221 0.00575
AFIX 13
H8 2 0.653469 0.690043 0.820535 10.83333 -1.20000
AFIX 0
O9 7 0.435701 0.613130 0.747280 11.00000 0.03540 0.03273 =
0.02921 -0.01558 -0.01557 0.00833
O10 7 0.431938 0.829016 0.703120 11.00000 0.05201 0.03442 =
0.03615 -0.01742 -0.02184 0.00837
O11 7 0.314649 0.723027 0.950009 11.00000 0.03308 0.03773 =
0.03551 -0.02149 -0.02001 0.01187
O12 7 0.171065 0.684473 0.831687 11.00000 0.03725 0.04651 =
0.05716 -0.02693 -0.02998 0.01322
CU1 4 0.900284 0.306189 0.771559 11.00000 0.04621 0.03693 =
0.03316 -0.01743 -0.02198 0.01462
CU2 4 0.500000 1.000000 0.500000 10.50000 0.03875 0.03996 =
0.04347 -0.02836 -0.02001 0.01396
O1W 7 0.947421 0.292342 0.902539 11.00000 0.03419 0.05214 =
0.03020 -0.01784 -0.01348 0.00728
AFIX 7
H1WA 2 1.023062 0.343428 0.878191 11.00000 -1.50000
H1WB 2 0.896136 0.261377 0.982525 11.00000 -1.50000
AFIX 0
PART 2
O1A 7 0.724027 0.983978 0.493292 10.50000 0.04361 0.04396 =
0.04772 -0.02535 -0.03379 0.02765
PART 0
O1F 7 0.903252 0.147076 0.821843 11.00000 0.06238 0.04379 =
0.07137 -0.02754 -0.03878 0.02181
PART 3
O2W 7 0.705540 0.988318 0.487769 10.50000 0.04822 0.04587 =
0.04958 -0.02798 -0.03175 0.02065
AFIX 7
H2WA 2 0.715395 0.920144 0.533053 10.50000 -1.50000
H2WB 2 0.733930 1.026779 0.513802 10.50000 -1.50000
AFIX 0
PART 0
O13 7 0.866354 0.460567 0.728308 11.00000 0.05159 0.03707 =
0.03404 -0.01872 -0.02454 0.01071
O14 7 0.818873 0.613409 0.591114 11.00000 0.05747 0.04548 =
0.04973 -0.02669 -0.03041 0.01867
O15 7 0.830749 0.668468 0.320738 11.00000 0.04057 0.03769 =
0.03237 -0.01042 -0.00867 0.01129
N1 6 0.853435 0.341343 0.632869 11.00000 0.03909 0.03014 =
0.03590 -0.01643 -0.01855 0.01317
N2 6 0.618725 0.625262 0.472915 11.00000 0.03253 0.03082 =
0.02563 -0.01079 -0.01098 0.00774
AFIX 43
H2 2 0.560706 0.572660 0.539864 11.00000 -1.20000
AFIX 0
N3 6 0.512409 0.897604 0.432674 11.00000 0.03946 0.02908 =
0.03524 -0.01727 -0.01809 0.00931
PART 1
N4 6 1.000789 -0.011079 0.860780 21.00000 0.06568 0.03807 =
0.09354 -0.02446 -0.03769 0.01583
PART 0
C6 1 0.819258 0.445418 0.580686 11.00000 0.02795 0.03619 =
0.02968 -0.01630 -0.00562 0.00170
C4 1 0.780576 0.486665 0.483030 11.00000 0.02548 0.02963 =
0.03085 -0.01248 -0.00798 0.00539
C3 1 0.783312 0.415576 0.436468 11.00000 0.04340 0.04435 =
0.03986 -0.02408 -0.02151 0.01383
AFIX 43
H3 2 0.762100 0.440292 0.369233 11.00000 -1.20000
AFIX 0
C2 1 0.817791 0.308969 0.491724 11.00000 0.05015 0.04466 =
0.05205 -0.03328 -0.02020 0.01156
AFIX 43
H2A 2 0.817618 0.260692 0.462762 11.00000 -1.20000
AFIX 0
C1 1 0.851848 0.274351 0.587841 11.00000 0.04183 0.04397 =
0.03940 -0.02579 -0.02480 0.01704
AFIX 43
H1 2 0.874883 0.202118 0.623995 11.00000 -1.20000
AFIX 0
C7 1 0.834533 0.515146 0.634825 11.00000 0.02659 0.03616 =
0.03522 -0.01963 -0.01248 0.00596
C5 1 0.745976 0.603502 0.418967 11.00000 0.03248 0.03889 =
0.02489 -0.01734 -0.01373 0.00873
C8 1 0.574814 0.734718 0.422472 11.00000 0.03273 0.02812 =
0.03142 -0.01174 -0.01232 0.00889
C12 1 0.557507 0.797331 0.475360 11.00000 0.03827 0.03711 =
0.03117 -0.01959 -0.01905 0.01055
AFIX 43
H12 2 0.577693 0.769492 0.543391 11.00000 -1.20000
AFIX 0
C11 1 0.480758 0.935432 0.334775 11.00000 0.05871 0.03558 =
0.03917 -0.01921 -0.03222 0.01867
AFIX 43
H11 2 0.443500 1.003060 0.307065 11.00000 -1.20000
AFIX 0
C10 1 0.500961 0.879166 0.275561 11.00000 0.07941 0.04293 =
0.03725 -0.02445 -0.03754 0.02759
AFIX 43
H10 2 0.482572 0.909692 0.206582 11.00000 -1.20000
AFIX 0
C9 1 0.549609 0.775007 0.319012 11.00000 0.06319 0.03970 =
0.04139 -0.02563 -0.03023 0.02041
AFIX 43
H9 2 0.564571 0.734195 0.280426 11.00000 -1.20000
AFIX 0
PART 1
C13 1 1.002660 0.097678 0.814066 21.00000 0.05343 0.04056 =
0.07560 -0.01098 -0.01488 0.01199
AFIX 43
H13 2 1.096382 0.141594 0.768316 21.00000 -1.20000
AFIX 0
PART 0
PART 2
N14 6 0.867213 -0.026228 0.937112 -21.00000 0.10498 0.05459 =
0.09513 -0.04274 -0.06310 0.04536
PART 0
PART 1
C15 1 1.131554 -0.058968 0.832485 21.00000 0.11177 0.06729 =
0.20380 -0.01712 0.00305 0.04641
AFIX 137
H15A 2 1.107500 -0.118608 0.820476 21.00000 -1.50000
H15B 2 1.168291 -0.088569 0.895271 21.00000 -1.50000
H15C 2 1.206651 -0.001872 0.762713 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C16 1 0.798545 1.065056 0.432996 10.50000 0.05618 0.06872 =
0.07308 -0.02341 -0.03320 0.01775
AFIX 93
H16A 2 0.760866 1.129345 0.392734 10.50000 -1.20000
H16B 2 0.899340 1.069442 0.422187 10.50000 -1.20000
AFIX 0
PART 0
PART -1
O2A 7 0.939007 1.081519 0.428681 10.50000 0.06130 0.09258 =
0.10345 -0.02113 -0.03683 0.00554
C17 1 0.928265 1.160916 0.347599 10.50000 0.05387 0.06993 =
0.08449 -0.02630 -0.03802 0.01520
PART 0
AFIX 6
O4W 7 0.082234 0.426844 1.154902 11.00000 0.03749 0.08820 =
0.06100 -0.04801 -0.00666 -0.01022
H4WA 2 0.065722 0.424161 1.219489 11.00000 -1.50000
H4WB 2 0.034915 0.368283 1.166950 11.00000 -1.50000
AFIX 6
O5W 7 0.786251 0.777632 0.661764 11.00000 0.06139 0.07816 =
0.08716 -0.05960 -0.02673 0.01195
H5WA 2 0.866135 0.755593 0.686463 11.00000 -1.50000
H5WB 2 0.764691 0.722122 0.649742 11.00000 -1.50000
AFIX 0
PART 1
C14 1 0.865852 -0.077943 0.958109 31.00000 0.06971 0.05054 =
0.09410 -0.00580 -0.04155 0.01308
AFIX 137
H14A 2 0.886455 -0.112891 1.028767 31.00000 -1.50000
H14B 2 0.829596 -0.135058 0.947473 31.00000 -1.50000
H14C 2 0.791789 -0.030334 0.962797 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C14A 1 0.921195 -0.070822 0.860865 -31.00000 0.25453 0.06029 =
0.10110 -0.04689 -0.04505 0.04358
AFIX 137
H14D 2 0.861420 -0.054386 0.813728 -31.00000 -1.50000
H14E 2 0.915528 -0.150952 0.906005 -31.00000 -1.50000
H14F 2 1.022932 -0.037111 0.811597 -31.00000 -1.50000
AFIX 0
C13A 1 0.856857 0.065840 0.909377 -21.00000 0.07819 0.05222 =
0.07625 -0.03924 -0.06385 0.04073
AFIX 43
H13A 2 0.799237 0.076806 0.970105 -21.00000 -1.20000
AFIX 0
C15A 1 0.800199 -0.114969 1.053991 -21.00000 0.11278 0.05564 =
0.09381 -0.04268 -0.06425 0.03547
AFIX 137
H15D 2 0.693748 -0.123651 1.075969 -21.00000 -1.50000
H15E 2 0.827718 -0.097454 1.104364 -21.00000 -1.50000
H15F 2 0.833803 -0.183827 1.060697 -21.00000 -1.50000
AFIX 0
PART 0
PART -1
H17A 2 0.987225 1.168256 0.277579 10.50000 -1.50000
H17B 2 0.837783 1.185162 0.360153 10.50000 -1.50000
HKLF 4
REM 20160913_sg01_0m_a.res in P-1
REM R1 = 0.0547 for 4327 Fo > 4sig(Fo) and 0.0664 for all 5309 data
REM 492 parameters refined using 98 restraints
END
WGHT 0.1258 0.0000
REM Instructions for potential hydrogen bonds
HTAB O5 O13
HTAB O7 O4W
HTAB O8 O5W
EQIV $2 x+1, y, z
HTAB O1W O16_$2
EQIV $3 -x+1, -y+1, -z+2
HTAB O1W O11_$3
HTAB O2W O5W
HTAB N2 O4
HTAB C1 O1F
HTAB C12 O9
EQIV $4 x, y+1, z-1
HTAB C11 O2_$4
EQIV $5 -x+1, -y+2, -z+1
HTAB C11 O10_$5
EQIV $6 -x+1, -y+1, -z+1
HTAB C9 O4_$6
EQIV $7 -x+2, -y+1, -z+1
HTAB C13 O15_$7
HTAB C16 O10_$5
HTAB O4W O13_$3
EQIV $8 -x, -y+1, -z+2
HTAB O4W O12_$8
HTAB O5W O4W_$3
HTAB O5W O14
EQIV $9 -x+1, -y, -z+2
HTAB C14 O3_$9
EQIV $10 -x+2, -y, -z+2
HTAB C15A O1W_$10
REM Highest difference peak 2.354, deepest hole -1.076, 1-sigma level 0.224
Q1 1 0.4383 0.2554 1.0604 11.00000 0.05 2.35
Q2 1 0.4603 0.4413 0.7795 11.00000 0.05 2.26
Q3 1 0.4347 0.6882 0.7677 11.00000 0.05 2.20
Q4 1 0.5994 0.2195 0.9692 11.00000 0.05 1.91
Q5 1 0.2918 0.4782 0.8651 11.00000 0.05 1.90
Q6 1 0.2820 0.4471 0.8922 11.00000 0.05 1.89
Q7 1 0.2593 0.7187 0.8679 11.00000 0.05 1.88
Q8 1 0.6214 0.2691 0.9400 11.00000 0.05 1.79
Q9 1 0.8034 0.2806 0.8398 11.00000 0.05 1.67
Q10 1 0.8141 0.3111 0.8207 11.00000 0.05 1.63
Q11 1 0.8570 0.0146 0.6715 11.00000 0.05 1.61
Q12 1 0.9758 0.2627 0.7383 11.00000 0.05 1.49
Q13 1 0.7048 0.2939 0.8807 11.00000 0.05 1.30
Q14 1 0.9953 0.3338 0.6975 11.00000 0.05 1.26
Q15 1 0.5854 0.9725 0.4627 11.00000 0.05 1.12
Q16 1 0.6605 0.7536 0.8807 11.00000 0.05 1.11
Q17 1 0.3993 0.4804 1.0670 11.00000 0.05 1.10
Q18 1 0.4132 0.5111 1.0472 11.00000 0.05 1.08
Q19 1 0.5992 1.0269 0.4300 11.00000 0.05 1.08
Q20 1 0.5354 0.6748 0.7192 11.00000 0.05 1.08
Q21 1 0.4181 0.5229 0.7800 11.00000 0.05 1.05
Q22 1 0.5557 0.4551 0.7195 11.00000 0.05 0.96
Q23 1 0.5017 0.4505 0.9203 11.00000 0.05 0.85
Q24 1 0.1998 0.4484 0.9422 11.00000 0.05 0.82
Q25 1 0.1771 0.6631 0.9418 11.00000 0.05 0.79
Q26 1 0.2875 0.5021 0.7727 11.00000 0.05 0.78
Q27 1 0.8538 0.3049 0.9469 11.00000 0.05 0.75
Q28 1 0.8252 0.7062 0.7067 11.00000 0.05 0.72
Q29 1 0.8184 0.2631 1.0882 11.00000 0.05 0.71
Q30 1 0.9154 0.3957 0.7252 11.00000 0.05 0.66
Q31 1 0.7835 0.3544 0.3436 11.00000 0.05 0.66
Q32 1 0.3795 0.7515 0.8883 11.00000 0.05 0.65
Q33 1 0.3952 0.5310 0.8896 11.00000 0.05 0.63
Q34 1 0.4826 0.6941 0.9121 11.00000 0.05 0.60
Q35 1 0.4198 0.2933 0.9100 11.00000 0.05 0.58
Q36 1 0.7447 0.6966 0.8650 11.00000 0.05 0.56
Q37 1 0.9437 1.1206 0.3362 11.00000 0.05 0.55
Q38 1 0.2535 0.7430 0.7575 11.00000 0.05 0.54
Q39 1 0.6765 0.4862 0.8879 11.00000 0.05 0.54
Q40 1 0.7530 0.5024 0.6023 11.00000 0.05 0.53
Q41 1 0.3624 0.4766 0.7437 11.00000 0.05 0.53
Q42 1 0.6814 0.6313 0.4510 11.00000 0.05 0.51
Q43 1 0.0046 0.4224 1.1386 11.00000 0.05 0.50
Q44 1 0.8560 0.2917 0.6309 11.00000 0.05 0.50
Q45 1 0.3643 0.8805 0.7190 11.00000 0.05 0.50
Q46 1 0.1039 0.5002 0.8610 11.00000 0.05 0.49
Q47 1 0.2524 0.4076 0.8161 11.00000 0.05 0.49
Q48 1 0.8914 0.4875 0.6871 11.00000 0.05 0.49
Q49 1 0.3720 0.3919 0.7559 11.00000 0.05 0.48
Q50 1 0.4775 0.9369 0.4361 11.00000 0.05 0.48
REM The information below was added by Olex2.
REM
REM R1 = 0.0547 for 4327 Fo > 4sig(Fo) and 0.0664 for all 11017 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.35, deepest hole -1.08
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0664
REM R1_gt = 0.0547
REM wR_ref = 0.1641
REM GOOF = 1.001
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 11017
REM Reflections_gt = 4327
REM Parameters = n/a
REM Hole = -1.08
REM Peak = 2.35
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_3
_database_code_depnum_ccdc_archive 'CCDC 1540699'
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_3
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W Check
RESPONSE: The hydrogen atoms associated with the solvate water molecule could not be located in the e-map.
;
_vrf_PLAT430_3
;
PROBLEM: Short Inter D...A Contact O5W .. O8W .. 2.73 Ang.
RESPONSE: There should be a strong hydrogen bond between the two atoms.
;
# end Validation Reply Form
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C24 H52 Cl Cr Cu3 Mo6 N6 O45'
_chemical_formula_weight 1998.42
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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 26.323(2)
_cell_length_b 9.8415(9)
_cell_length_c 25.627(3)
_cell_angle_alpha 90
_cell_angle_beta 117.9220(10)
_cell_angle_gamma 90
_cell_volume 5865.9(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 3446
_cell_measurement_theta_min 2.26
_cell_measurement_theta_max 25.55
_exptl_crystal_description block
_exptl_crystal_colour blue
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 2.263
_exptl_crystal_F_000 3912
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.080
_exptl_absorpt_coefficient_mu 2.638
_shelx_estimated_absorpt_T_min 0.648
_shelx_estimated_absorpt_T_max 0.817
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6417
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0491 before and 0.0362 after correction. The Ratio of minimum to maximum transmission is 0.8610. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 16311
_diffrn_reflns_av_unetI/netI 0.0514
_diffrn_reflns_av_R_equivalents 0.0474
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 1.751
_diffrn_reflns_theta_max 25.844
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 5652
_reflns_number_gt 4118
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'SAINT v8.34A (Bruker, 2013)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+11.3172P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 5652
_refine_ls_number_parameters 412
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0659
_refine_ls_R_factor_gt 0.0388
_refine_ls_wR_factor_ref 0.1000
_refine_ls_wR_factor_gt 0.0891
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_restrained_S_all 1.032
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.50190(2) 0.73479(5) 0.40692(2) 0.02515(14) Uani 1 1 d . . . . .
Mo2 Mo 0.61569(2) 0.69709(5) 0.53807(2) 0.02482(14) Uani 1 1 d . . . . .
Mo3 Mo 0.61282(2) 0.46566(5) 0.63277(2) 0.02457(14) Uani 1 1 d . . . . .
Cu1 Cu 0.5000 0.73031(11) 0.2500 0.0305(3) Uani 1 2 d S T P . .
Cu2 Cu 0.71451(3) 0.22661(8) 0.60932(3) 0.03118(19) Uani 1 1 d . . . . .
Cr1 Cr 0.5000 0.5000 0.5000 0.0180(3) Uani 1 2 d S . P . .
Cl1 Cl 0.5000 0.9623(3) 0.2500 0.0716(9) Uani 1 2 d S T P . .
O1 O 0.76073(19) 0.4810(5) 0.41852(19) 0.0423(11) Uani 1 1 d . . . . .
O1W O 0.5000 0.5200(7) 0.2500 0.0560(19) Uani 1 2 d S T P . .
H1WA H 0.5358 0.4851 0.2673 0.084 Uiso 0.5 1 d R U P . .
H1WB H 0.4855 0.4851 0.2133 0.084 Uiso 0.5 1 d R U P . .
O2 O 0.65483(18) 0.3667(5) 0.44625(19) 0.0404(11) Uani 1 1 d . . . . .
O2W O 0.77066(19) 0.1780(5) 0.69056(19) 0.0473(12) Uani 1 1 d . . . . .
H2WA H 0.7923 0.2468 0.7077 0.071 Uiso 1 1 d R U . . .
H2WB H 0.7943 0.1178 0.6903 0.071 Uiso 1 1 d R U . . .
O3 O 0.65894(16) 0.2758(4) 0.52770(18) 0.0309(10) Uani 1 1 d . . . . .
O3W O 0.65715(16) 0.1104(4) 0.61701(18) 0.0341(10) Uani 1 1 d . . . . .
H3WA H 0.6442 0.0488 0.5895 0.051 Uiso 1 1 d R U . . .
H3WB H 0.6269 0.1576 0.6099 0.051 Uiso 1 1 d R U . . .
O4 O 0.68018(16) 0.4098(4) 0.64761(17) 0.0345(10) Uani 1 1 d . . . . .
O5 O 0.61588(19) 0.4935(4) 0.69925(18) 0.0391(11) Uani 1 1 d . . . . .
O6 O 0.61548(16) 0.6522(4) 0.61158(16) 0.0276(9) Uani 1 1 d . . . . .
O7 O 0.51630(15) 0.4905(4) 0.58329(15) 0.0216(8) Uani 1 1 d . . . . .
H7 H 0.4988 0.5594 0.5975 0.026 Uiso 1 1 calc R U . . .
O8 O 0.68201(16) 0.6420(5) 0.55081(18) 0.0388(11) Uani 1 1 d . . . . .
O9 O 0.62111(19) 0.8682(4) 0.5473(2) 0.0418(11) Uani 1 1 d . . . . .
O10 O 0.58048(16) 0.6813(4) 0.45312(16) 0.0274(9) Uani 1 1 d . . . . .
O11 O 0.51735(16) 0.6954(4) 0.50079(16) 0.0238(8) Uani 1 1 d . . . . .
H11 H 0.5003 0.7585 0.5178 0.029 Uiso 1 1 calc R U . . .
O12 O 0.41666(14) 0.5242(4) 0.46738(15) 0.0211(8) Uani 1 1 d . . . . .
H12 H 0.4026 0.5936 0.4849 0.025 Uiso 1 1 calc R U . . .
O13 O 0.50645(19) 0.9057(4) 0.4167(2) 0.0421(11) Uani 1 1 d . . . . .
O14 O 0.42230(16) 0.7149(4) 0.38771(17) 0.0266(9) Uani 1 1 d . . . . .
O15 O 0.49767(17) 0.7072(5) 0.33950(17) 0.0365(10) Uani 1 1 d . . . . .
N1 N 0.5863(2) 0.7281(5) 0.2933(2) 0.0320(12) Uani 1 1 d . . . . .
N2 N 0.7039(2) 0.6231(5) 0.4362(2) 0.0328(12) Uani 1 1 d . . . . .
H2 H 0.6955 0.6558 0.4624 0.039 Uiso 1 1 calc R U . . .
N3 N 0.7665(2) 0.3464(5) 0.5923(2) 0.0290(11) Uani 1 1 d . . . . .
C1 C 0.6161(2) 0.6769(6) 0.3483(3) 0.0303(14) Uani 1 1 d . . . . .
H1 H 0.5960 0.6422 0.3670 0.036 Uiso 1 1 calc R U . . .
C2 C 0.6162(3) 0.7769(7) 0.2672(3) 0.0372(16) Uani 1 1 d . . . . .
H2A H 0.5961 0.8143 0.2296 0.045 Uiso 1 1 calc R U . . .
C3 C 0.6752(3) 0.7743(7) 0.2934(3) 0.0426(17) Uani 1 1 d . . . . .
H3 H 0.6943 0.8073 0.2733 0.051 Uiso 1 1 calc R U . . .
C4 C 0.7056(3) 0.7225(7) 0.3495(3) 0.0356(15) Uani 1 1 d . . . . .
H4 H 0.7456 0.7198 0.3680 0.043 Uiso 1 1 calc R U . . .
C5 C 0.6754(2) 0.6743(6) 0.3779(2) 0.0269(13) Uani 1 1 d . . . . .
C6 C 0.7438(2) 0.5246(6) 0.4518(3) 0.0295(14) Uani 1 1 d . . . . .
C7 C 0.7697(2) 0.4753(6) 0.5147(3) 0.0281(13) Uani 1 1 d . . . . .
C8 C 0.8264(3) 0.5096(6) 0.5527(3) 0.0373(15) Uani 1 1 d . . . . .
H8 H 0.8472 0.5626 0.5394 0.045 Uiso 1 1 calc R U . . .
C9 C 0.8513(3) 0.4655(7) 0.6095(3) 0.0418(16) Uani 1 1 d . . . . .
H9 H 0.8890 0.4896 0.6355 0.050 Uiso 1 1 calc R U . . .
C10 C 0.8203(3) 0.3845(7) 0.6285(3) 0.0393(16) Uani 1 1 d . . . . .
H10 H 0.8375 0.3558 0.6676 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7411(2) 0.3918(6) 0.5359(2) 0.0264(13) Uani 1 1 d . . . . .
C12 C 0.6802(2) 0.3415(6) 0.4993(3) 0.0285(13) Uani 1 1 d . . . . .
O4W O 0.7376(3) -0.0136(7) 0.7367(3) 0.093(2) Uani 1 1 d G . . . .
H4WA H 0.7667 -0.0477 0.7660 0.140 Uiso 1 1 d G U . . .
H4WB H 0.7125 -0.0750 0.7198 0.140 Uiso 1 1 d G U . . .
O5W O 0.6425(4) -0.1741(8) 0.7052(3) 0.127(3) Uani 1 1 d . . . . .
O6W O 0.6127(6) 0.6291(15) 0.7957(7) 0.107(5) Uani 0.5 1 d . . P . .
O7W O 0.4644(3) 0.6344(6) 0.6333(3) 0.0750(18) Uani 1 1 d G . . . .
H7WA H 0.4323 0.6596 0.6052 0.113 Uiso 1 1 d G U . . .
H7WB H 0.4807 0.7078 0.6504 0.113 Uiso 1 1 d G U . . .
O8W O 0.5294(6) 0.8766(12) 0.6722(5) 0.091(4) Uani 0.5 1 d . . P . .
O9W O 0.4527(3) 0.8476(7) 0.5296(4) 0.090(2) Uani 1 1 d G . . . .
H9WA H 0.4522 0.9220 0.5462 0.135 Uiso 1 1 d G U . . .
H9WB H 0.4191 0.8134 0.5131 0.135 Uiso 1 1 d G U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0239(3) 0.0276(3) 0.0252(3) 0.0019(2) 0.0126(2) -0.0008(2)
Mo2 0.0202(3) 0.0270(3) 0.0272(3) -0.0048(2) 0.0111(2) -0.0058(2)
Mo3 0.0212(3) 0.0285(3) 0.0216(3) -0.0024(2) 0.0080(2) 0.0008(2)
Cu1 0.0207(5) 0.0415(6) 0.0268(5) 0.000 0.0089(4) 0.000
Cu2 0.0248(4) 0.0359(4) 0.0322(4) 0.0014(3) 0.0128(3) 0.0019(3)
Cr1 0.0154(6) 0.0192(6) 0.0196(6) -0.0018(5) 0.0084(5) -0.0012(5)
Cl1 0.0544(18) 0.0431(16) 0.099(2) 0.000 0.0202(17) 0.000
O1 0.046(3) 0.046(3) 0.047(3) 0.005(2) 0.032(2) 0.017(2)
O1W 0.047(5) 0.052(5) 0.053(5) 0.000 0.010(4) 0.000
O2 0.029(2) 0.050(3) 0.033(3) 0.004(2) 0.006(2) -0.007(2)
O2W 0.039(3) 0.049(3) 0.044(3) 0.002(2) 0.010(2) 0.000(2)
O3 0.023(2) 0.036(2) 0.035(2) 0.001(2) 0.0138(19) -0.0007(18)
O3W 0.028(2) 0.030(2) 0.044(3) -0.003(2) 0.017(2) 0.0044(18)
O4 0.022(2) 0.042(3) 0.031(2) -0.005(2) 0.0053(18) 0.0030(18)
O5 0.050(3) 0.037(3) 0.028(2) -0.004(2) 0.017(2) 0.001(2)
O6 0.026(2) 0.028(2) 0.028(2) -0.0075(18) 0.0116(18) -0.0042(17)
O7 0.019(2) 0.025(2) 0.0222(19) -0.0024(17) 0.0116(16) 0.0011(16)
O8 0.017(2) 0.058(3) 0.037(2) -0.006(2) 0.0090(19) -0.003(2)
O9 0.047(3) 0.032(2) 0.050(3) -0.009(2) 0.026(2) -0.013(2)
O10 0.024(2) 0.036(2) 0.027(2) -0.0003(19) 0.0153(18) -0.0028(17)
O11 0.025(2) 0.021(2) 0.028(2) -0.0035(17) 0.0143(18) -0.0001(16)
O12 0.018(2) 0.0208(19) 0.027(2) -0.0029(17) 0.0124(17) -0.0004(15)
O13 0.049(3) 0.028(2) 0.050(3) 0.001(2) 0.024(2) -0.005(2)
O14 0.024(2) 0.025(2) 0.030(2) 0.0024(18) 0.0120(18) 0.0064(17)
O15 0.026(2) 0.055(3) 0.029(2) 0.005(2) 0.0130(19) 0.001(2)
N1 0.024(3) 0.046(3) 0.026(3) -0.001(2) 0.012(2) -0.001(2)
N2 0.029(3) 0.039(3) 0.030(3) 0.000(2) 0.014(2) 0.009(2)
N3 0.026(3) 0.031(3) 0.027(3) -0.001(2) 0.010(2) 0.000(2)
C1 0.027(3) 0.040(4) 0.032(3) 0.003(3) 0.020(3) 0.003(3)
C2 0.032(4) 0.053(4) 0.024(3) 0.003(3) 0.012(3) -0.007(3)
C3 0.033(4) 0.058(5) 0.039(4) 0.005(4) 0.019(3) -0.008(3)
C4 0.019(3) 0.046(4) 0.036(4) -0.004(3) 0.008(3) -0.006(3)
C5 0.023(3) 0.028(3) 0.027(3) -0.004(3) 0.010(3) 0.000(2)
C6 0.021(3) 0.032(3) 0.035(3) -0.001(3) 0.013(3) 0.000(3)
C7 0.023(3) 0.027(3) 0.035(3) -0.001(3) 0.014(3) 0.007(2)
C8 0.028(4) 0.036(4) 0.048(4) 0.003(3) 0.018(3) -0.003(3)
C9 0.024(4) 0.046(4) 0.043(4) -0.001(3) 0.006(3) -0.006(3)
C10 0.027(4) 0.050(4) 0.028(3) 0.002(3) 0.001(3) 0.001(3)
C11 0.019(3) 0.027(3) 0.030(3) -0.003(3) 0.009(3) 0.002(2)
C12 0.023(3) 0.031(3) 0.030(3) -0.004(3) 0.010(3) 0.005(3)
O4W 0.062(4) 0.119(6) 0.063(4) 0.045(4) 0.000(3) -0.014(4)
O5W 0.190(9) 0.105(6) 0.088(5) -0.050(5) 0.066(6) -0.068(6)
O6W 0.127(13) 0.097(11) 0.132(12) -0.056(10) 0.089(11) -0.029(9)
O7W 0.055(4) 0.079(4) 0.085(4) -0.032(4) 0.027(3) 0.004(3)
O8W 0.150(13) 0.060(8) 0.068(8) -0.016(7) 0.057(9) -0.014(8)
O9W 0.060(4) 0.073(5) 0.131(6) -0.042(4) 0.040(4) -0.011(3)
_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
Mo1 O13 1.697(4) . ?
Mo1 O15 1.700(4) . ?
Mo1 O10 1.914(4) . ?
Mo1 O14 1.925(4) . ?
Mo1 O11 2.277(4) . ?
Mo1 O7 2.307(4) 5_666 ?
Mo2 O9 1.697(4) . ?
Mo2 O8 1.707(4) . ?
Mo2 O10 1.932(4) . ?
Mo2 O6 1.937(4) . ?
Mo2 O11 2.302(4) . ?
Mo2 O12 2.319(4) 5_666 ?
Mo3 O5 1.690(4) . ?
Mo3 O4 1.721(4) . ?
Mo3 O6 1.925(4) . ?
Mo3 O14 1.958(4) 5_666 ?
Mo3 O7 2.259(3) . ?
Mo3 O12 2.310(3) 5_666 ?
Cu1 N1 2.007(5) . ?
Cu1 N1 2.007(5) 2_655 ?
Cu1 O1W 2.070(7) . ?
Cu1 Cl1 2.283(3) . ?
Cu1 O15 2.334(4) 2_655 ?
Cu1 O15 2.334(4) . ?
Cu2 O2W 1.966(4) . ?
Cu2 O3 1.971(4) . ?
Cu2 O3W 1.976(4) . ?
Cu2 N3 2.003(5) . ?
Cu2 O1 2.355(4) 7_656 ?
Cu2 O4 2.420(4) . ?
Cr1 O12 1.962(3) . ?
Cr1 O12 1.962(3) 5_666 ?
Cr1 O7 1.973(3) 5_666 ?
Cr1 O7 1.973(3) . ?
Cr1 O11 1.974(4) . ?
Cr1 O11 1.974(4) 5_666 ?
O1 C6 1.211(7) . ?
O1 Cu2 2.355(4) 7_656 ?
O2 C12 1.226(7) . ?
O3 C12 1.282(7) . ?
O7 Mo1 2.307(4) 5_666 ?
O12 Mo3 2.310(3) 5_666 ?
O12 Mo2 2.319(3) 5_666 ?
O14 Mo3 1.958(4) 5_666 ?
N1 C2 1.338(7) . ?
N1 C1 1.350(7) . ?
N2 C6 1.345(7) . ?
N2 C5 1.415(7) . ?
N3 C10 1.333(7) . ?
N3 C11 1.354(7) . ?
C1 C5 1.380(8) . ?
C2 C3 1.374(8) . ?
C3 C4 1.375(9) . ?
C4 C5 1.390(8) . ?
C6 C7 1.506(8) . ?
C7 C11 1.388(8) . ?
C7 C8 1.388(8) . ?
C8 C9 1.358(9) . ?
C9 C10 1.381(9) . ?
C11 C12 1.512(8) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Mo1 O15 106.0(2) . . ?
O13 Mo1 O10 101.54(19) . . ?
O15 Mo1 O10 97.03(17) . . ?
O13 Mo1 O14 97.55(19) . . ?
O15 Mo1 O14 100.28(18) . . ?
O10 Mo1 O14 149.54(16) . . ?
O13 Mo1 O11 92.71(18) . . ?
O15 Mo1 O11 160.15(18) . . ?
O10 Mo1 O11 72.13(14) . . ?
O14 Mo1 O11 83.53(14) . . ?
O13 Mo1 O7 160.17(17) . 5_666 ?
O15 Mo1 O7 92.24(17) . 5_666 ?
O10 Mo1 O7 83.57(15) . 5_666 ?
O14 Mo1 O7 70.95(14) . 5_666 ?
O11 Mo1 O7 70.43(12) . 5_666 ?
O9 Mo2 O8 106.1(2) . . ?
O9 Mo2 O10 101.63(19) . . ?
O8 Mo2 O10 95.62(18) . . ?
O9 Mo2 O6 97.39(19) . . ?
O8 Mo2 O6 102.12(18) . . ?
O10 Mo2 O6 149.21(16) . . ?
O9 Mo2 O11 94.00(17) . . ?
O8 Mo2 O11 158.08(18) . . ?
O10 Mo2 O11 71.27(14) . . ?
O6 Mo2 O11 83.53(14) . . ?
O9 Mo2 O12 160.87(17) . 5_666 ?
O8 Mo2 O12 91.56(18) . 5_666 ?
O10 Mo2 O12 83.56(15) . 5_666 ?
O6 Mo2 O12 71.12(14) . 5_666 ?
O11 Mo2 O12 70.02(12) . 5_666 ?
O5 Mo3 O4 105.7(2) . . ?
O5 Mo3 O6 97.97(18) . . ?
O4 Mo3 O6 101.39(18) . . ?
O5 Mo3 O14 102.20(19) . 5_666 ?
O4 Mo3 O14 94.43(18) . 5_666 ?
O6 Mo3 O14 149.88(16) . 5_666 ?
O5 Mo3 O7 93.36(17) . . ?
O4 Mo3 O7 158.48(16) . . ?
O6 Mo3 O7 85.32(14) . . ?
O14 Mo3 O7 71.47(14) 5_666 . ?
O5 Mo3 O12 161.07(17) . 5_666 ?
O4 Mo3 O12 91.99(16) . 5_666 ?
O6 Mo3 O12 71.52(14) . 5_666 ?
O14 Mo3 O12 82.56(14) 5_666 5_666 ?
O7 Mo3 O12 70.57(12) . 5_666 ?
N1 Cu1 N1 178.7(3) . 2_655 ?
N1 Cu1 O1W 89.37(15) . . ?
N1 Cu1 O1W 89.37(15) 2_655 . ?
N1 Cu1 Cl1 90.63(15) . . ?
N1 Cu1 Cl1 90.63(15) 2_655 . ?
O1W Cu1 Cl1 180.0 . . ?
N1 Cu1 O15 89.91(16) . 2_655 ?
N1 Cu1 O15 89.96(16) 2_655 2_655 ?
O1W Cu1 O15 84.42(11) . 2_655 ?
Cl1 Cu1 O15 95.58(11) . 2_655 ?
N1 Cu1 O15 89.97(17) . . ?
N1 Cu1 O15 89.91(16) 2_655 . ?
O1W Cu1 O15 84.42(11) . . ?
Cl1 Cu1 O15 95.58(11) . . ?
O15 Cu1 O15 168.8(2) 2_655 . ?
O2W Cu2 O3 179.35(18) . . ?
O2W Cu2 O3W 89.10(18) . . ?
O3 Cu2 O3W 91.50(17) . . ?
O2W Cu2 N3 97.0(2) . . ?
O3 Cu2 N3 82.40(18) . . ?
O3W Cu2 N3 173.84(18) . . ?
O2W Cu2 O1 86.12(19) . 7_656 ?
O3 Cu2 O1 93.72(16) . 7_656 ?
O3W Cu2 O1 81.99(16) . 7_656 ?
N3 Cu2 O1 97.49(17) . 7_656 ?
O2W Cu2 O4 89.44(18) . . ?
O3 Cu2 O4 90.85(15) . . ?
O3W Cu2 O4 86.73(16) . . ?
N3 Cu2 O4 94.18(17) . . ?
O1 Cu2 O4 167.94(15) 7_656 . ?
O12 Cr1 O12 180.0(2) . 5_666 ?
O12 Cr1 O7 84.26(14) . 5_666 ?
O12 Cr1 O7 95.75(14) 5_666 5_666 ?
O12 Cr1 O7 95.74(14) . . ?
O12 Cr1 O7 84.26(14) 5_666 . ?
O7 Cr1 O7 180.0 5_666 . ?
O12 Cr1 O11 95.35(15) . . ?
O12 Cr1 O11 84.65(15) 5_666 . ?
O7 Cr1 O11 84.09(15) 5_666 . ?
O7 Cr1 O11 95.91(15) . . ?
O12 Cr1 O11 84.65(15) . 5_666 ?
O12 Cr1 O11 95.35(15) 5_666 5_666 ?
O7 Cr1 O11 95.91(15) 5_666 5_666 ?
O7 Cr1 O11 84.09(15) . 5_666 ?
O11 Cr1 O11 180.0 . 5_666 ?
C6 O1 Cu2 140.0(4) . 7_656 ?
C12 O3 Cu2 115.0(4) . . ?
Mo3 O4 Cu2 133.7(2) . . ?
Mo3 O6 Mo2 120.57(19) . . ?
Cr1 O7 Mo3 103.30(14) . . ?
Cr1 O7 Mo1 102.25(15) . 5_666 ?
Mo3 O7 Mo1 94.09(13) . 5_666 ?
Mo1 O10 Mo2 118.95(19) . . ?
Cr1 O11 Mo1 103.24(15) . . ?
Cr1 O11 Mo2 102.77(15) . . ?
Mo1 O11 Mo2 92.70(13) . . ?
Cr1 O12 Mo3 101.86(14) . 5_666 ?
Cr1 O12 Mo2 102.57(15) . 5_666 ?
Mo3 O12 Mo2 92.91(13) 5_666 5_666 ?
Mo1 O14 Mo3 118.78(18) . 5_666 ?
Mo1 O15 Cu1 164.5(3) . . ?
C2 N1 C1 117.7(5) . . ?
C2 N1 Cu1 119.9(4) . . ?
C1 N1 Cu1 122.4(4) . . ?
C6 N2 C5 121.6(5) . . ?
C10 N3 C11 118.9(5) . . ?
C10 N3 Cu2 128.8(4) . . ?
C11 N3 Cu2 112.3(4) . . ?
N1 C1 C5 122.4(5) . . ?
N1 C2 C3 123.0(6) . . ?
C2 C3 C4 119.3(6) . . ?
C3 C4 C5 118.5(6) . . ?
C1 C5 C4 119.0(5) . . ?
C1 C5 N2 119.3(5) . . ?
C4 C5 N2 121.7(5) . . ?
O1 C6 N2 122.7(6) . . ?
O1 C6 C7 120.4(5) . . ?
N2 C6 C7 116.7(5) . . ?
C11 C7 C8 118.1(6) . . ?
C11 C7 C6 123.6(5) . . ?
C8 C7 C6 118.3(5) . . ?
C9 C8 C7 119.8(6) . . ?
C8 C9 C10 119.5(6) . . ?
N3 C10 C9 121.9(6) . . ?
N3 C11 C7 121.8(5) . . ?
N3 C11 C12 113.9(5) . . ?
C7 C11 C12 124.3(5) . . ?
O2 C12 O3 125.1(6) . . ?
O2 C12 C11 119.4(5) . . ?
O3 C12 C11 115.4(5) . . ?
_refine_diff_density_max 1.092
_refine_diff_density_min -0.794
_refine_diff_density_rms 0.135
_shelx_res_file
;
111.res created by SHELXL-2014/7
TITL 111_a.res in C2/c
REM Old TITL 111 in C2/c
REM SHELXT solution in C2/c
REM R1 0.114, Rweak 0.003, Alpha 0.036, Orientation as input
REM Formula found by SHELXT: N37 O37 Cu4 Mo6
CELL 0.71073 26.3226 9.8415 25.627 90 117.922 90
ZERR 4 0.0023 0.0009 0.0033 0 0.001 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cl Cr Cu Mo N O
UNIT 96 208 4 4 12 24 24 180
L.S. 14
PLAN 20
SIZE 0.08 0.15 0.18
TEMP 23
bump
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.047700 11.317201
FVAR 0.09305
MO1 6 0.501905 0.734792 0.406924 11.00000 0.02389 0.02763 =
0.02525 0.00188 0.01260 -0.00080
MO2 6 0.615692 0.697089 0.538073 11.00000 0.02023 0.02703 =
0.02720 -0.00476 0.01112 -0.00579
MO3 6 0.612816 0.465665 0.632770 11.00000 0.02124 0.02846 =
0.02161 -0.00238 0.00801 0.00084
CU1 5 0.500000 0.730311 0.250000 10.50000 0.02071 0.04148 =
0.02677 0.00000 0.00892 0.00000
CU2 5 0.714511 0.226610 0.609324 11.00000 0.02484 0.03590 =
0.03219 0.00140 0.01285 0.00185
CR1 4 0.500000 0.500000 0.500000 10.50000 0.01542 0.01922 =
0.01962 -0.00179 0.00838 -0.00123
CL1 3 0.500000 0.962334 0.250000 10.50000 0.05439 0.04306 =
0.09866 0.00000 0.02019 0.00000
O1 8 0.760729 0.481033 0.418524 11.00000 0.04613 0.04584 =
0.04715 0.00522 0.03202 0.01654
O1W 8 0.500000 0.519988 0.250000 10.50000 0.04654 0.05215 =
0.05314 0.00000 0.00994 0.00000
AFIX 7
H1WA 2 0.535782 0.485113 0.267276 10.50000 -1.50000
H1WB 2 0.485532 0.485113 0.213335 10.50000 -1.50000
AFIX 0
O2 8 0.654830 0.366698 0.446251 11.00000 0.02878 0.04989 =
0.03256 0.00433 0.00592 -0.00679
O2W 8 0.770656 0.178005 0.690555 11.00000 0.03864 0.04856 =
0.04354 0.00180 0.01000 -0.00003
AFIX 7
H2WA 2 0.792267 0.246847 0.707679 11.00000 -1.50000
H2WB 2 0.794255 0.117765 0.690253 11.00000 -1.50000
AFIX 0
O3 8 0.658945 0.275842 0.527700 11.00000 0.02309 0.03553 =
0.03455 0.00063 0.01382 -0.00066
O3W 8 0.657151 0.110375 0.617009 11.00000 0.02814 0.03038 =
0.04381 -0.00300 0.01678 0.00435
AFIX 7
H3WA 2 0.644156 0.048809 0.589539 11.00000 -1.50000
H3WB 2 0.626872 0.157592 0.609934 11.00000 -1.50000
AFIX 0
O4 8 0.680183 0.409757 0.647610 11.00000 0.02169 0.04206 =
0.03128 -0.00467 0.00532 0.00302
O5 8 0.615881 0.493547 0.699252 11.00000 0.05034 0.03742 =
0.02824 -0.00385 0.01743 0.00108
O6 8 0.615482 0.652225 0.611583 11.00000 0.02570 0.02782 =
0.02813 -0.00747 0.01164 -0.00416
O7 8 0.516304 0.490500 0.583293 11.00000 0.01949 0.02525 =
0.02224 -0.00241 0.01156 0.00109
AFIX 13
H7 2 0.498811 0.559366 0.597482 11.00000 -1.20000
AFIX 0
O8 8 0.682009 0.642036 0.550813 11.00000 0.01718 0.05830 =
0.03652 -0.00615 0.00896 -0.00269
O9 8 0.621114 0.868217 0.547327 11.00000 0.04709 0.03248 =
0.04955 -0.00949 0.02564 -0.01254
O10 8 0.580484 0.681329 0.453120 11.00000 0.02366 0.03629 =
0.02658 -0.00030 0.01530 -0.00278
O11 8 0.517348 0.695399 0.500787 11.00000 0.02478 0.02125 =
0.02775 -0.00347 0.01431 -0.00014
AFIX 13
H11 2 0.500338 0.758518 0.517835 11.00000 -1.20000
AFIX 0
O12 8 0.416664 0.524193 0.467382 11.00000 0.01817 0.02077 =
0.02657 -0.00287 0.01244 -0.00043
AFIX 13
H12 2 0.402611 0.593641 0.484880 11.00000 -1.20000
AFIX 0
O13 8 0.506452 0.905714 0.416714 11.00000 0.04933 0.02844 =
0.04956 0.00082 0.02390 -0.00509
O14 8 0.422300 0.714944 0.387714 11.00000 0.02401 0.02546 =
0.02974 0.00244 0.01198 0.00635
O15 8 0.497667 0.707234 0.339495 11.00000 0.02603 0.05470 =
0.02891 0.00521 0.01304 0.00078
N1 7 0.586257 0.728060 0.293278 11.00000 0.02444 0.04571 =
0.02586 -0.00059 0.01181 -0.00104
N2 7 0.703891 0.623116 0.436222 11.00000 0.02931 0.03940 =
0.02982 0.00036 0.01388 0.00929
AFIX 43
H2 2 0.695505 0.655793 0.462367 11.00000 -1.20000
AFIX 0
N3 7 0.766526 0.346380 0.592336 11.00000 0.02556 0.03108 =
0.02721 -0.00089 0.00965 0.00040
C1 1 0.616113 0.676930 0.348348 11.00000 0.02683 0.03955 =
0.03172 0.00302 0.01959 0.00341
AFIX 43
H1 2 0.595978 0.642248 0.367047 11.00000 -1.20000
AFIX 0
C2 1 0.616154 0.776926 0.267196 11.00000 0.03243 0.05283 =
0.02446 0.00266 0.01170 -0.00742
AFIX 43
H2A 2 0.596076 0.814344 0.229638 11.00000 -1.20000
AFIX 0
C3 1 0.675177 0.774347 0.293373 11.00000 0.03323 0.05801 =
0.03894 0.00521 0.01878 -0.00771
AFIX 43
H3 2 0.694317 0.807333 0.273343 11.00000 -1.20000
AFIX 0
C4 1 0.705648 0.722525 0.349459 11.00000 0.01911 0.04624 =
0.03614 -0.00350 0.00849 -0.00607
AFIX 43
H4 2 0.745610 0.719801 0.367984 11.00000 -1.20000
AFIX 0
C5 1 0.675405 0.674296 0.377861 11.00000 0.02298 0.02777 =
0.02726 -0.00419 0.00963 -0.00046
C6 1 0.743754 0.524625 0.451775 11.00000 0.02148 0.03164 =
0.03536 -0.00112 0.01331 0.00043
C7 1 0.769749 0.475315 0.514654 11.00000 0.02291 0.02736 =
0.03507 -0.00066 0.01435 0.00663
C8 1 0.826393 0.509583 0.552730 11.00000 0.02797 0.03559 =
0.04800 0.00261 0.01758 -0.00258
AFIX 43
H8 2 0.847200 0.562605 0.539376 11.00000 -1.20000
AFIX 0
C9 1 0.851339 0.465456 0.609538 11.00000 0.02430 0.04623 =
0.04264 -0.00136 0.00556 -0.00609
AFIX 43
H9 2 0.889028 0.489560 0.635490 11.00000 -1.20000
AFIX 0
C10 1 0.820343 0.384510 0.628515 11.00000 0.02704 0.04987 =
0.02758 0.00154 0.00150 0.00145
AFIX 43
H10 2 0.837506 0.355804 0.667637 11.00000 -1.20000
AFIX 0
C11 1 0.741081 0.391843 0.535916 11.00000 0.01865 0.02684 =
0.03014 -0.00326 0.00854 0.00151
C12 1 0.680210 0.341491 0.499256 11.00000 0.02267 0.03053 =
0.02966 -0.00415 0.01017 0.00533
AFIX 6
O4W 8 0.737639 -0.013600 0.736721 11.00000 0.06233 0.11926 =
0.06319 0.04489 0.00038 -0.01446
H4WA 2 0.766679 -0.047687 0.766018 11.00000 -1.50000
H4WB 2 0.712521 -0.075013 0.719802 11.00000 -1.50000
AFIX 0
O5W 8 0.642480 -0.174117 0.705207 11.00000 0.19048 0.10475 =
0.08766 -0.04955 0.06604 -0.06790
O6W 8 0.612659 0.629063 0.795747 10.50000 0.12666 0.09745 =
0.13172 -0.05594 0.08915 -0.02887
AFIX 6
O7W 8 0.464360 0.634394 0.633290 11.00000 0.05507 0.07871 =
0.08490 -0.03218 0.02747 0.00434
H7WA 2 0.432321 0.659573 0.605208 11.00000 -1.50000
H7WB 2 0.480684 0.707787 0.650373 11.00000 -1.50000
AFIX 0
O8W 8 0.529371 0.876603 0.672186 10.50000 0.15046 0.05961 =
0.06844 -0.01627 0.05681 -0.01448
AFIX 6
O9W 8 0.452694 0.847624 0.529645 11.00000 0.05964 0.07291 =
0.13146 -0.04181 0.03972 -0.01135
H9WA 2 0.452187 0.922008 0.546224 11.00000 -1.50000
H9WB 2 0.419123 0.813407 0.513137 11.00000 -1.50000
AFIX 0
HKLF 4
REM 111_a.res in C2/c
REM R1 = 0.0388 for 4118 Fo > 4sig(Fo) and 0.0659 for all 5652 data
REM 412 parameters refined using 2 restraints
END
WGHT 0.0501 9.4451
REM Highest difference peak 1.092, deepest hole -0.794, 1-sigma level 0.135
Q1 1 0.4965 0.8158 0.5305 11.00000 0.05 1.09
Q2 1 0.5940 -0.1235 0.6900 11.00000 0.05 0.95
Q3 1 0.5935 0.6994 0.4960 11.00000 0.05 0.75
Q4 1 0.5035 0.7416 0.4412 11.00000 0.05 0.61
Q5 1 0.5480 0.7726 0.7254 11.00000 0.05 0.60
Q6 1 0.5707 0.6808 0.7656 11.00000 0.05 0.57
Q7 1 0.4981 0.9656 0.1897 11.00000 0.05 0.55
Q8 1 0.4922 0.7366 0.3666 11.00000 0.05 0.54
Q9 1 0.6108 0.6858 0.7738 11.00000 0.05 0.54
Q10 1 0.5345 0.8215 0.7034 11.00000 0.05 0.54
Q11 1 0.8301 0.2813 0.7088 11.00000 0.05 0.52
Q12 1 0.6538 0.5987 0.5517 11.00000 0.05 0.51
Q13 1 0.7759 0.8346 0.3291 11.00000 0.05 0.51
Q14 1 0.4294 0.5579 0.4490 11.00000 0.05 0.49
Q15 1 0.6871 0.4837 0.6446 11.00000 0.05 0.49
Q16 1 0.5778 0.7977 0.5003 11.00000 0.05 0.49
Q17 1 0.6249 0.4632 0.6707 11.00000 0.05 0.48
Q18 1 0.6000 0.7167 0.4633 11.00000 0.05 0.48
Q19 1 0.5910 0.5140 0.6613 11.00000 0.05 0.47
Q20 1 0.5917 0.6187 0.8131 11.00000 0.05 0.46
;
_shelx_res_checksum 9036