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#$Date: 2021-07-15 12:51:38 +0300 (Thu, 15 Jul 2021) $
#$Revision: 267559 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/41/1564173.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1564173
loop_
_publ_author_name
'Bruno, Sofia M.'
'Amarante, Tatiana R.'
'Almeida Paz, Filipe A.'
'Pillinger, Martyn'
'Valente, Anabela A.'
'Gonçalves, Isabel S.'
_publ_section_title
;
 Oxidation of sulfides in aqueous media catalyzed by
 pyrazole-oxidoperoxido-molybdenum(VI) complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119814
_journal_paper_doi               10.1016/j.ica.2020.119814
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C10 H16 Mo8 N4 O26.20, 4(C5 H9 N2), 4(H2 O)'
_chemical_formula_sum            'C30 H60 Mo8 N12 O30.2'
_chemical_formula_weight         1839.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                115.385(2)
_cell_angle_beta                 91.606(2)
_cell_angle_gamma                108.6980(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6007(4)
_cell_length_b                   13.1512(7)
_cell_length_c                   14.6215(7)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.54
_cell_volume                     1388.58(12)
_computing_cell_refinement       'SAINT V8.37a   (Bruker, 2015)'
_computing_data_collection       'APEX3 2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37a   (Bruker, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       'ω / φ scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26732
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         3.574
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2016/2
  Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
  J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       Block
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.1044
_exptl_transmission_factor_min   0.0661
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0201P)²+0.6616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0444
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7001
_reflns_number_total             7440
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-511-119814.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C30 H60 Mo8 N12 O30.20'
_cod_database_code               1564173
_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.
;
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.733
_exptl_absorpt_special_details
;
?
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.38675(2) 0.37091(2) 0.20416(2) 0.01432(3) Uani 1 1 d . . . . .
Mo2 Mo 0.49059(2) 0.23010(2) 0.31737(2) 0.01372(3) Uani 1 1 d . . . . .
Mo3 Mo 0.66900(2) 0.37190(2) 0.56037(2) 0.01390(3) Uani 1 1 d . . . . .
Mo4 Mo 0.34681(2) 0.45360(2) 0.56262(2) 0.01230(3) Uani 1 1 d . . . . .
O1 O 0.19951(15) 0.35821(11) 0.14951(10) 0.0233(2) Uani 1 1 d . . . . .
O2 O 0.47263(16) 0.29723(11) 0.10393(9) 0.0220(2) Uani 1 1 d . . . . .
O3 O 0.31462(14) 0.25673(10) 0.25482(9) 0.0166(2) Uani 1 1 d . . . . .
O4 O 0.47245(13) 0.37866(10) 0.46433(8) 0.0136(2) Uani 1 1 d . . . . .
O5 O 0.68991(14) 0.28563(10) 0.41859(9) 0.0163(2) Uani 1 1 d . . . . .
O6 O 0.56663(15) 0.15681(11) 0.21268(9) 0.0215(2) Uani 1 1 d . . . . .
O7 O 0.35860(15) 0.11672(10) 0.33993(10) 0.0202(2) Uani 1 1 d . . . . .
O8 O 0.86461(18) 0.42070(14) 0.63178(13) 0.0214(3) Uani 0.9 1 d . . P A .
O14 O 0.8875(15) 0.3759(11) 0.5725(9) 0.022(2) Uiso 0.1 1 d D . P A 1
O15 O 0.8480(18) 0.4571(12) 0.6662(10) 0.021(3) Uiso 0.1 1 d D . P A 1
O9 O 0.55441(16) 0.24952(11) 0.57486(10) 0.0215(2) Uani 1 1 d . . . . .
O10 O 0.57711(14) 0.48652(10) 0.65246(8) 0.0156(2) Uani 1 1 d . . . . .
O11 O 0.37722(14) 0.59383(10) 0.68746(8) 0.0155(2) Uani 1 1 d . . . . .
O12 O 0.21467(14) 0.46645(10) 0.47737(9) 0.0157(2) Uani 1 1 d . . . . .
O13 O 0.22014(15) 0.33823(10) 0.58088(9) 0.0198(2) Uani 1 1 d . . . . .
N1 N 0.52765(18) 0.53008(13) 0.17578(11) 0.0182(3) Uani 1 1 d . . . . .
N2 N 0.68152(18) 0.54128(13) 0.15075(11) 0.0195(3) Uani 1 1 d D . . . .
H2 H 0.739(3) 0.4979(18) 0.1635(17) 0.029 Uiso 1 1 d D U . . .
N3 N 0.06683(18) -0.05606(13) 0.62596(12) 0.0217(3) Uani 1 1 d D . . . .
H3 H 0.050(3) -0.1272(14) 0.6309(18) 0.033 Uiso 1 1 d D U . . .
N4 N -0.05750(19) -0.01370(14) 0.62913(12) 0.0230(3) Uani 1 1 d D . . . .
H4 H -0.1674(16) -0.0648(18) 0.6223(19) 0.035 Uiso 1 1 d D U . . .
N5 N 0.83269(19) 0.19135(13) 0.08843(11) 0.0219(3) Uani 1 1 d D . . . .
H5 H 0.854(3) 0.2739(10) 0.1254(16) 0.033 Uiso 1 1 d D U . . .
N6 N 0.89414(19) 0.14077(13) 0.13614(11) 0.0221(3) Uani 1 1 d D . . . .
H6 H 0.943(3) 0.1827(19) 0.2056(9) 0.033 Uiso 1 1 d D U . . .
C3 C 0.3162(2) 0.61940(17) 0.16658(15) 0.0259(4) Uani 1 1 d . . . . .
H3A H 0.333769 0.689731 0.233419 0.039 Uiso 1 1 calc R U . . .
H3B H 0.235460 0.546924 0.166126 0.039 Uiso 1 1 calc R U . . .
H3C H 0.272750 0.632573 0.111569 0.039 Uiso 1 1 calc R U . . .
C4 C 0.4778(2) 0.60266(15) 0.14931(13) 0.0201(3) Uani 1 1 d . . . . .
C5 C 0.6000(2) 0.65789(16) 0.10698(14) 0.0231(3) Uani 1 1 d . . . . .
H5A H 0.595251 0.712273 0.081300 0.028 Uiso 1 1 calc R U . . .
C6 C 0.7289(2) 0.61796(15) 0.10980(13) 0.0212(3) Uani 1 1 d . . . . .
C7 C 0.8959(2) 0.64722(19) 0.07963(16) 0.0292(4) Uani 1 1 d . . . . .
H7A H 0.945335 0.589208 0.078450 0.044 Uiso 1 1 calc R U . . .
H7B H 0.969495 0.729299 0.129725 0.044 Uiso 1 1 calc R U . . .
H7C H 0.882371 0.642354 0.010922 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3727(2) 0.00978(18) 0.63157(17) 0.0292(4) Uani 1 1 d . . . . .
H8A H 0.412946 0.020590 0.699715 0.044 Uiso 1 1 calc R U . . .
H8B H 0.454885 0.069236 0.616564 0.044 Uiso 1 1 calc R U . . .
H8C H 0.357254 -0.072116 0.579092 0.044 Uiso 1 1 calc R U . . .
C9 C 0.2105(2) 0.02744(15) 0.63058(13) 0.0207(3) Uani 1 1 d . . . . .
C10 C 0.1742(2) 0.12507(16) 0.63530(14) 0.0221(3) Uani 1 1 d . . . . .
H10A H 0.250977 0.197490 0.638481 0.027 Uiso 1 1 calc R U . . .
C11 C 0.0040(2) 0.09625(16) 0.63447(13) 0.0223(3) Uani 1 1 d . . . . .
C12 C -0.1049(3) 0.1661(2) 0.63907(16) 0.0317(4) Uani 1 1 d . . . . .
H12A H -0.222640 0.112131 0.620149 0.047 Uiso 1 1 calc R U . . .
H12B H -0.080730 0.200089 0.590821 0.047 Uiso 1 1 calc R U . . .
H12C H -0.082901 0.231835 0.709272 0.047 Uiso 1 1 calc R U . . .
C13 C 0.6568(3) 0.13437(18) -0.07421(15) 0.0298(4) Uani 1 1 d . . . . .
H13A H 0.674856 0.220768 -0.040242 0.045 Uiso 1 1 calc R U . . .
H13B H 0.536486 0.086581 -0.092106 0.045 Uiso 1 1 calc R U . . .
H13C H 0.703784 0.114750 -0.137115 0.045 Uiso 1 1 calc R U . . .
C14 C 0.7403(2) 0.10558(16) -0.00325(13) 0.0223(3) Uani 1 1 d . . . . .
C15 C 0.7447(2) -0.00431(16) -0.01463(14) 0.0262(4) Uani 1 1 d . . . . .
H15 H 0.691820 -0.081498 -0.072778 0.031 Uiso 1 1 calc R U . . .
C16 C 0.8412(2) 0.02118(15) 0.07543(13) 0.0230(3) Uani 1 1 d . . . . .
C17 C 0.8866(3) -0.06011(18) 0.10820(16) 0.0321(4) Uani 1 1 d . . . . .
H17A H 1.002655 -0.019779 0.145893 0.048 Uiso 1 1 calc R U . . .
H17B H 0.874893 -0.135410 0.047177 0.048 Uiso 1 1 calc R U . . .
H17C H 0.812136 -0.078587 0.153086 0.048 Uiso 1 1 calc R U . . .
O1W O -0.03731(14) 0.25498(10) 0.34900(9) 0.0185(2) Uani 1 1 d D . . . .
H1X H 0.0564(15) 0.3263(13) 0.3846(15) 0.028 Uiso 1 1 d D U . . .
H1Y H -0.1340(15) 0.2672(18) 0.3710(16) 0.028 Uiso 1 1 d D U . . .
O2W O 0.86662(15) 0.42278(11) 0.20583(9) 0.0196(2) Uani 1 1 d D . . . .
H2X H 0.9696(14) 0.4730(17) 0.2511(13) 0.029 Uiso 1 1 d D U . . .
H2Y H 0.7808(17) 0.4112(19) 0.2423(14) 0.029 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 Mo1 O2 105.99(6) . .
O1 Mo1 O3 100.61(5) . .
O2 Mo1 O3 100.73(5) . .
O1 Mo1 O10 100.03(5) . 2_666
O2 Mo1 O10 148.07(5) . 2_666
O3 Mo1 O10 92.20(5) . 2_666
O1 Mo1 N1 91.90(5) . .
O2 Mo1 N1 81.78(5) . .
O3 Mo1 N1 165.92(5) . .
O10 Mo1 N1 79.16(5) 2_666 .
O1 Mo1 O11 167.47(5) . 2_666
O2 Mo1 O11 86.43(5) . 2_666
O3 Mo1 O11 74.92(4) . 2_666
O10 Mo1 O11 68.81(4) 2_666 2_666
N1 Mo1 O11 91.50(4) . 2_666
O6 Mo2 O7 104.71(6) . .
O6 Mo2 O3 101.59(5) . .
O7 Mo2 O3 96.00(5) . .
O6 Mo2 O5 95.79(5) . .
O7 Mo2 O5 100.07(5) . .
O3 Mo2 O5 152.46(5) . .
O6 Mo2 O4 160.30(5) . .
O7 Mo2 O4 93.30(5) . .
O3 Mo2 O4 84.09(4) . .
O5 Mo2 O4 72.85(4) . .
O6 Mo2 O11 89.61(5) . 2_666
O7 Mo2 O11 164.73(5) . 2_666
O3 Mo2 O11 75.59(4) . 2_666
O5 Mo2 O11 83.40(4) . 2_666
O4 Mo2 O11 73.39(4) . 2_666
O9 Mo3 O8 104.19(6) . .
O9 Mo3 O15 105.9(5) . .
O8 Mo3 O15 18.9(4) . .
O9 Mo3 O14 104.6(4) . .
O8 Mo3 O14 28.2(3) . .
O15 Mo3 O14 46.8(3) . .
O9 Mo3 O5 97.71(5) . .
O8 Mo3 O5 104.66(7) . .
O15 Mo3 O5 122.3(4) . .
O14 Mo3 O5 76.7(4) . .
O9 Mo3 O10 97.97(5) . .
O8 Mo3 O10 101.90(7) . .
O15 Mo3 O10 83.1(4) . .
O14 Mo3 O10 128.8(4) . .
O5 Mo3 O10 144.63(5) . .
O9 Mo3 O4 99.54(5) . .
O8 Mo3 O4 156.18(6) . .
O15 Mo3 O4 146.8(4) . .
O14 Mo3 O4 144.0(4) . .
O5 Mo3 O4 73.88(4) . .
O10 Mo3 O4 72.36(4) . .
O9 Mo3 O12 170.30(5) . 2_666
O8 Mo3 O12 85.51(6) . 2_666
O15 Mo3 O12 83.3(5) . 2_666
O14 Mo3 O12 83.8(4) . 2_666
O5 Mo3 O12 79.41(4) . 2_666
O10 Mo3 O12 79.84(4) . 2_666
O4 Mo3 O12 70.78(4) . 2_666
O13 Mo4 O12 103.68(6) . .
O13 Mo4 O11 104.36(5) . .
O12 Mo4 O11 101.83(5) . .
O13 Mo4 O4 103.36(5) . .
O12 Mo4 O4 97.60(5) . .
O11 Mo4 O4 141.02(5) . .
O13 Mo4 O10 98.17(5) . .
O12 Mo4 O10 157.89(5) . .
O11 Mo4 O10 75.54(5) . .
O4 Mo4 O10 73.85(4) . .
O13 Mo4 O4 179.32(5) . 2_666
O12 Mo4 O4 75.71(4) . 2_666
O11 Mo4 O4 75.52(4) . 2_666
O4 Mo4 O4 77.05(4) . 2_666
O10 Mo4 O4 82.45(4) . 2_666
Mo1 O3 Mo2 115.93(6) . .
Mo4 O4 Mo3 103.81(5) . .
Mo4 O4 Mo2 152.33(6) . .
Mo3 O4 Mo2 93.76(4) . .
Mo4 O4 Mo4 102.95(4) . 2_666
Mo3 O4 Mo4 96.96(4) . 2_666
Mo2 O4 Mo4 95.82(4) . 2_666
Mo3 O5 Mo2 114.20(5) . .
O15 O8 O14 166.5(17) . .
O15 O8 Mo3 89.5(15) . .
O14 O8 Mo3 84.8(8) . .
O8 O14 O15 5.4(7) . .
O8 O14 Mo3 67.0(7) . .
O15 O14 Mo3 64.8(7) . .
O8 O15 O14 8.1(10) . .
O8 O15 Mo3 71.7(13) . .
O14 O15 Mo3 68.4(7) . .
Mo3 O10 Mo1 146.17(6) . 2_666
Mo3 O10 Mo4 105.69(5) . .
Mo1 O10 Mo4 108.06(5) 2_666 .
Mo4 O11 Mo2 114.27(5) . 2_666
Mo4 O11 Mo1 107.26(5) . 2_666
Mo2 O11 Mo1 90.12(4) 2_666 2_666
Mo4 O12 Mo3 116.22(5) . 2_666
C4 N1 N2 105.35(13) . .
C4 N1 Mo1 132.81(11) . .
N2 N1 Mo1 119.00(10) . .
C6 N2 N1 111.88(14) . .
C6 N2 H2 129.2(14) . .
N1 N2 H2 119.0(14) . .
C9 N3 N4 108.98(14) . .
C9 N3 H3 129.1(15) . .
N4 N3 H3 121.2(15) . .
C11 N4 N3 109.42(14) . .
C11 N4 H4 131.9(15) . .
N3 N4 H4 118.5(15) . .
C14 N5 N6 109.33(14) . .
C14 N5 H5 133.1(14) . .
N6 N5 H5 117.4(14) . .
C16 N6 N5 109.28(14) . .
C16 N6 H6 127.2(15) . .
N5 N6 H6 122.1(15) . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C4 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 C5 109.83(15) . .
N1 C4 C3 122.79(15) . .
C5 C4 C3 127.37(15) . .
C6 C5 C4 106.43(15) . .
C6 C5 H5A 126.8 . .
C4 C5 H5A 126.8 . .
N2 C6 C5 106.51(15) . .
N2 C6 C7 121.23(16) . .
C5 C6 C7 132.24(16) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 C10 107.41(15) . .
N3 C9 C8 122.37(15) . .
C10 C9 C8 130.22(16) . .
C11 C10 C9 106.73(15) . .
C11 C10 H10A 126.6 . .
C9 C10 H10A 126.6 . .
N4 C11 C10 107.46(15) . .
N4 C11 C12 121.58(17) . .
C10 C11 C12 130.96(17) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 H13A 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C14 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N5 C14 C15 107.41(16) . .
N5 C14 C13 121.66(16) . .
C15 C14 C13 130.92(17) . .
C16 C15 C14 106.55(15) . .
C16 C15 H15 126.7 . .
C14 C15 H15 126.7 . .
N6 C16 C15 107.41(15) . .
N6 C16 C17 121.80(16) . .
C15 C16 C17 130.79(16) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
H1X O1W H1Y 110.3(12) . .
H2X O2W H2Y 110.7(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.7032(12) .
Mo1 O2 1.7130(12) .
Mo1 O3 1.8896(11) .
Mo1 O10 2.0558(11) 2_666
Mo1 N1 2.2735(14) .
Mo1 O11 2.3309(11) 2_666
Mo2 O6 1.7015(12) .
Mo2 O7 1.7258(12) .
Mo2 O3 1.9458(11) .
Mo2 O5 1.9470(11) .
Mo2 O4 2.2524(11) .
Mo2 O11 2.2619(11) 2_666
Mo3 O9 1.7011(12) .
Mo3 O8 1.7225(14) .
Mo3 O15 1.815(14) .
Mo3 O14 1.864(12) .
Mo3 O5 1.9370(11) .
Mo3 O10 1.9476(11) .
Mo3 O4 2.2154(11) .
Mo3 O12 2.3448(11) 2_666
Mo4 O13 1.6924(11) .
Mo4 O12 1.7602(11) .
Mo4 O11 1.8919(11) .
Mo4 O4 1.9391(11) .
Mo4 O10 2.1572(11) .
Mo4 O4 2.4534(11) 2_666
O8 O15 0.587(11) .
O8 O14 0.885(11) .
O14 O15 1.462(9) .
N1 C4 1.347(2) .
N1 N2 1.3621(19) .
N2 C6 1.345(2) .
N2 H2 0.933(9) .
N3 C9 1.342(2) .
N3 N4 1.349(2) .
N3 H3 0.934(9) .
N4 C11 1.337(2) .
N4 H4 0.941(10) .
N5 C14 1.330(2) .
N5 N6 1.346(2) .
N5 H5 0.932(9) .
N6 C16 1.338(2) .
N6 H6 0.928(9) .
C3 C4 1.488(2) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.396(2) .
C5 C6 1.377(2) .
C5 H5A 0.9500 .
C6 C7 1.494(3) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.486(2) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.391(2) .
C10 C11 1.388(2) .
C10 H10A 0.9500 .
C11 C12 1.492(3) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.485(3) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.395(2) .
C15 C16 1.384(3) .
C15 H15 0.9500 .
C16 C17 1.491(2) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O1W H1X 0.934(9) .
O1W H1Y 0.937(9) .
O2W H2X 0.936(9) .
O2W H2Y 0.934(9) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O2W 0.933(9) 1.936(10) 2.8648(18) 173(2) . yes
N3 H3 O1W 0.934(9) 1.797(10) 2.7280(18) 174(2) 2_556 yes
N4 H4 O7 0.941(10) 1.769(13) 2.6624(19) 157(2) 2_556 yes
N5 H5 O2W 0.932(9) 1.763(10) 2.6867(19) 171(2) . yes
N6 H6 O1W 0.928(9) 1.871(12) 2.7589(19) 160(2) 1_655 yes
C3 H3A O9 0.98 2.62 3.384(2) 135.0 2_666 yes
C3 H3B O1 0.98 2.30 3.148(2) 143.9 . yes
C3 H3B O15a 0.98 2.59 3.222(14) 122.1 2_666 yes
C7 H7C O1 0.98 2.43 3.392(2) 168.4 2_665 yes
C8 H8B O9 0.98 2.59 3.496(2) 154.3 . yes
C10 H10A O13 0.95 2.42 3.141(2) 132.8 . yes
C12 H12B O14a 0.98 2.53 3.314(12) 136.4 1_455 yes
C15 H15 O2 0.95 2.56 3.312(2) 136.6 2_655 yes
C15 H15 O3 0.95 2.66 3.526(2) 152.6 2_655 yes
C15 H15 O6 0.95 2.59 3.274(2) 129.3 2_655 yes
O1W H1X O12 0.934(9) 1.799(11) 2.7177(16) 167.2(19) . yes
O1W H1Y O5 0.937(9) 1.728(9) 2.6628(16) 175(2) 1_455 yes
O1W H1Y O14a 0.937(9) 2.64(2) 3.154(12) 115.5(15) 1_455 yes
O2W H2X O8 0.936(9) 1.858(11) 2.7694(19) 163.8(18) 2_766 yes
O2W H2X O14a 0.936(9) 2.444(19) 3.264(12) 146.3(16) 2_766 yes
O2W H2X O15a 0.936(9) 1.669(17) 2.597(14) 171(2) 2_766 yes
O2W H2Y O11 0.934(9) 1.728(10) 2.6575(16) 173(2) 2_666 yes
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
O1 Mo1 O3 Mo2 175.84(7) . . . .
O2 Mo1 O3 Mo2 67.14(7) . . . .
O10 Mo1 O3 Mo2 -83.52(6) 2_666 . . .
N1 Mo1 O3 Mo2 -31.9(2) . . . .
O11 Mo1 O3 Mo2 -16.16(5) 2_666 . . .
O9 Mo3 O8 O15 -97.7(15) . . . .
O14 Mo3 O8 O15 167.7(17) . . . .
O5 Mo3 O8 O15 160.2(15) . . . .
O10 Mo3 O8 O15 3.8(15) . . . .
O4 Mo3 O8 O15 77.0(15) . . . .
O12 Mo3 O8 O15 82.4(15) 2_666 . . .
O9 Mo3 O8 O14 94.6(8) . . . .
O15 Mo3 O8 O14 -167.7(17) . . . .
O5 Mo3 O8 O14 -7.5(8) . . . .
O10 Mo3 O8 O14 -163.9(8) . . . .
O4 Mo3 O8 O14 -90.7(8) . . . .
O12 Mo3 O8 O14 -85.3(8) 2_666 . . .
Mo3 O8 O14 O15 66(7) . . . .
O15 O8 O14 Mo3 -66(7) . . . .
O9 Mo3 O14 O8 -92.8(7) . . . .
O15 Mo3 O14 O8 5.4(7) . . . .
O5 Mo3 O14 O8 172.6(8) . . . .
O10 Mo3 O14 O8 20.4(10) . . . .
O4 Mo3 O14 O8 136.7(5) . . . .
O12 Mo3 O14 O8 92.0(7) 2_666 . . .
O9 Mo3 O14 O15 -98.2(7) . . . .
O8 Mo3 O14 O15 -5.4(7) . . . .
O5 Mo3 O14 O15 167.1(8) . . . .
O10 Mo3 O14 O15 14.9(9) . . . .
O4 Mo3 O14 O15 131.2(7) . . . .
O12 Mo3 O14 O15 86.6(7) 2_666 . . .
Mo3 O8 O15 O14 -65(7) . . . .
O14 O8 O15 Mo3 65(7) . . . .
Mo3 O14 O15 O8 112(7) . . . .
O8 O14 O15 Mo3 -112(7) . . . .
O9 Mo3 O15 O8 87.4(14) . . . .
O14 Mo3 O15 O8 -7.9(11) . . . .
O5 Mo3 O15 O8 -22.8(17) . . . .
O10 Mo3 O15 O8 -176.3(15) . . . .
O4 Mo3 O15 O8 -134.1(10) . . . .
O12 Mo3 O15 O8 -95.7(14) 2_666 . . .
O9 Mo3 O15 O14 95.3(7) . . . .
O8 Mo3 O15 O14 7.9(11) . . . .
O5 Mo3 O15 O14 -14.8(9) . . . .
O10 Mo3 O15 O14 -168.3(7) . . . .
O4 Mo3 O15 O14 -126.2(7) . . . .
O12 Mo3 O15 O14 -87.8(7) 2_666 . . .
O13 Mo4 O11 Mo2 -171.15(6) . . . 2_666
O12 Mo4 O11 Mo2 -63.51(6) . . . 2_666
O4 Mo4 O11 Mo2 54.77(9) . . . 2_666
O10 Mo4 O11 Mo2 93.94(6) . . . 2_666
O4 Mo4 O11 Mo2 8.16(4) 2_666 . . 2_666
O13 Mo4 O11 Mo1 90.65(6) . . . 2_666
O12 Mo4 O11 Mo1 -161.71(5) . . . 2_666
O4 Mo4 O11 Mo1 -43.43(9) . . . 2_666
O10 Mo4 O11 Mo1 -4.26(4) . . . 2_666
O4 Mo4 O11 Mo1 -90.04(5) 2_666 . . 2_666
O13 Mo4 O12 Mo3 175.00(6) . . . 2_666
O11 Mo4 O12 Mo3 66.83(6) . . . 2_666
O4 Mo4 O12 Mo3 -79.20(6) . . . 2_666
O10 Mo4 O12 Mo3 -13.85(16) . . . 2_666
O4 Mo4 O12 Mo3 -4.70(5) 2_666 . . 2_666
C4 N1 N2 C6 -0.01(18) . . . .
Mo1 N1 N2 C6 163.29(11) . . . .
C9 N3 N4 C11 0.8(2) . . . .
C14 N5 N6 C16 -0.20(19) . . . .
N2 N1 C4 C5 0.57(19) . . . .
Mo1 N1 C4 C5 -159.39(12) . . . .
N2 N1 C4 C3 -178.35(16) . . . .
Mo1 N1 C4 C3 21.7(2) . . . .
N1 C4 C5 C6 -0.9(2) . . . .
C3 C4 C5 C6 177.94(17) . . . .
N1 N2 C6 C5 -0.56(19) . . . .
N1 N2 C6 C7 178.04(15) . . . .
C4 C5 C6 N2 0.87(19) . . . .
C4 C5 C6 C7 -177.51(19) . . . .
N4 N3 C9 C10 -0.9(2) . . . .
N4 N3 C9 C8 178.31(16) . . . .
N3 C9 C10 C11 0.7(2) . . . .
C8 C9 C10 C11 -178.44(19) . . . .
N3 N4 C11 C10 -0.3(2) . . . .
N3 N4 C11 C12 -179.93(16) . . . .
C9 C10 C11 N4 -0.2(2) . . . .
C9 C10 C11 C12 179.35(19) . . . .
N6 N5 C14 C15 -0.6(2) . . . .
N6 N5 C14 C13 -179.57(16) . . . .
N5 C14 C15 C16 1.1(2) . . . .
C13 C14 C15 C16 179.98(19) . . . .
N5 N6 C16 C15 0.9(2) . . . .
N5 N6 C16 C17 -178.98(17) . . . .
C14 C15 C16 N6 -1.2(2) . . . .
C14 C15 C16 C17 178.64(19) . . . .
