#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:48:18 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232265 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/73/4347320.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_4347320
loop_
_publ_author_name
'Wang, Yang'
'Li, Bao'
'Qian, Hujun'
'Wu, Lixin'
_publ_section_title
;
 Controlled Triol-Derivative Bonding and Decoration Transformation on
 Cu-Centered Anderson-Evans Polyoxometalates.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4271
_journal_page_last               4277
_journal_paper_doi               10.1021/acs.inorgchem.6b00008
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C10 H20 Cu Mo6 O26, 2(C16 H36 N), 2(C2 H4 O2)'
_chemical_formula_sum            'C46 H100 Cu Mo6 N2 O30'
_chemical_formula_weight         1800.46
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.229(3)
_cell_length_b                   10.440(2)
_cell_length_c                   22.333(5)
_cell_measurement_reflns_used    28710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.13
_cell_volume                     3301.0(12)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30913
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.8643
_exptl_absorpt_correction_T_min  0.8287
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1822
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                6301
_reflns_number_total             7546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00008_si_002.cif
_cod_data_source_block           3a
_cod_original_cell_volume        3301.1(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347320
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0222(2) 0.2684(3) 0.02624(14) 0.0305(6) Uani 1 1 d . . .
H1A H -0.0520 0.3490 0.0140 0.037 Uiso 1 1 calc R . .
H1B H 0.0453 0.2780 0.0245 0.037 Uiso 1 1 calc R . .
C2 C -0.1464(2) 0.2259(3) 0.09875(15) 0.0357(7) Uani 1 1 d . . .
H2A H -0.1544 0.2145 0.1411 0.043 Uiso 1 1 calc R . .
H2B H -0.1782 0.3046 0.0855 0.043 Uiso 1 1 calc R . .
C3 C 0.0158(2) 0.1222(3) 0.11705(13) 0.0307(6) Uani 1 1 d . A .
H3A H 0.0823 0.1363 0.1130 0.037 Uiso 1 1 calc R . .
H3B H 0.0085 0.1139 0.1596 0.037 Uiso 1 1 calc R . .
C4 C -0.0412(2) 0.2391(3) 0.09160(13) 0.0303(6) Uani 1 1 d . . .
C5 C -0.0005(5) 0.3513(7) 0.1304(4) 0.0448(18) Uani 0.842(7) 1 d PD A 1
H5A H -0.0012 0.3304 0.1727 0.054 Uiso 0.842(7) 1 calc PR A 1
H5B H 0.0645 0.3666 0.1227 0.054 Uiso 0.842(7) 1 calc PR A 1
O13 O -0.0556(3) 0.4636(3) 0.1165(2) 0.0746(15) Uani 0.842(7) 1 d PD A 1
H13 H -0.0204 0.5242 0.1118 0.112 Uiso 0.842(7) 1 calc PR A 1
C5' C -0.0215(16) 0.369(4) 0.130(2) 0.028(8) Uiso 0.158(7) 1 d PD A 2
H5'1 H -0.0523 0.4411 0.1083 0.033 Uiso 0.158(7) 1 calc PR A 2
H5'2 H -0.0453 0.3619 0.1686 0.033 Uiso 0.158(7) 1 calc PR A 2
O13' O 0.0771(11) 0.3861(13) 0.1362(9) 0.048(5) Uani 0.158(7) 1 d PD A 2
H13' H 0.1029 0.3177 0.1454 0.072 Uiso 0.158(7) 1 calc PR A 2
C6 C 0.4357(2) 0.0668(3) 0.21804(15) 0.0369(7) Uani 1 1 d . . .
H6A H 0.4523 0.0136 0.2532 0.044 Uiso 1 1 calc R . .
H6B H 0.4364 0.1552 0.2314 0.044 Uiso 1 1 calc R . .
C7 C 0.3358(2) 0.0333(4) 0.19235(15) 0.0407(7) Uani 1 1 d . . .
H7A H 0.3327 -0.0568 0.1816 0.049 Uiso 1 1 calc R . .
H7B H 0.3191 0.0829 0.1561 0.049 Uiso 1 1 calc R . .
C8 C 0.2659(3) 0.0610(4) 0.23790(18) 0.0476(9) Uani 1 1 d . . .
H8A H 0.2077 0.0150 0.2262 0.057 Uiso 1 1 calc R . .
H8B H 0.2915 0.0290 0.2769 0.057 Uiso 1 1 calc R . .
C9 C 0.2435(3) 0.2022(5) 0.2435(3) 0.0742(15) Uani 1 1 d . . .
H9A H 0.3013 0.2501 0.2493 0.111 Uiso 1 1 calc R . .
H9B H 0.2079 0.2151 0.2773 0.111 Uiso 1 1 calc R . .
H9C H 0.2071 0.2308 0.2075 0.111 Uiso 1 1 calc R . .
C10 C 0.6083(2) 0.0622(4) 0.20928(19) 0.0476(9) Uani 1 1 d . . .
H10A H 0.6555 0.0430 0.1821 0.057 Uiso 1 1 calc R . .
H10B H 0.6137 -0.0025 0.2406 0.057 Uiso 1 1 calc R . .
C11 C 0.6319(3) 0.1912(4) 0.2382(3) 0.0695(14) Uani 1 1 d . . .
H11A H 0.5867 0.2111 0.2666 0.083 Uiso 1 1 calc R . .
H11B H 0.6279 0.2573 0.2076 0.083 Uiso 1 1 calc R . .
C12 C 0.7317(3) 0.1886(5) 0.2710(2) 0.0660(14) Uani 1 1 d . . .
H12A H 0.7760 0.1668 0.2423 0.079 Uiso 1 1 calc R . .
H12B H 0.7475 0.2738 0.2862 0.079 Uiso 1 1 calc R . .
C13 C 0.7431(4) 0.0960(6) 0.3219(3) 0.0875(18) Uani 1 1 d . . .
H13A H 0.6898 0.1021 0.3449 0.131 Uiso 1 1 calc R . .
H13B H 0.7998 0.1157 0.3472 0.131 Uiso 1 1 calc R . .
H13C H 0.7472 0.0107 0.3064 0.131 Uiso 1 1 calc R . .
C14 C 0.4944(3) 0.1497(3) 0.12539(18) 0.0477(9) Uani 1 1 d . . .
H14A H 0.4317 0.1359 0.1051 0.057 Uiso 1 1 calc R B 1
H14B H 0.4946 0.2335 0.1442 0.057 Uiso 1 1 calc R B 1
C15 C 0.5639(4) 0.1521(5) 0.0782(3) 0.0836(18) Uani 0.50 1 d PD C 1
H15A H 0.5502 0.0842 0.0490 0.100 Uiso 0.50 1 calc PR C 1
H15B H 0.6281 0.1417 0.0967 0.100 Uiso 0.50 1 calc PR C 1
C16 C 0.5509(16) 0.2846(14) 0.0479(7) 0.106(8) Uani 0.50 1 d PD C 1
H16A H 0.5370 0.3506 0.0763 0.127 Uiso 0.50 1 calc PR C 1
H16B H 0.6056 0.3094 0.0279 0.127 Uiso 0.50 1 calc PR C 1
C17 C 0.4693(12) 0.256(2) 0.0049(6) 0.126(6) Uani 0.50 1 d PD C 1
H17A H 0.4834 0.1834 -0.0191 0.188 Uiso 0.50 1 calc PR C 1
H17B H 0.4551 0.3286 -0.0206 0.188 Uiso 0.50 1 calc PR C 1
H17C H 0.4158 0.2364 0.0264 0.188 Uiso 0.50 1 calc PR C 1
C15' C 0.5639(4) 0.1521(5) 0.0782(3) 0.0836(18) Uani 0.50 1 d PD C 2
H15C H 0.5676 0.0673 0.0609 0.100 Uiso 0.50 1 calc PR C 2
H15D H 0.6261 0.1738 0.0973 0.100 Uiso 0.50 1 calc PR C 2
C16' C 0.5356(10) 0.2503(11) 0.0269(6) 0.059(4) Uani 0.50 1 d PD C 2
H16C H 0.5694 0.2309 -0.0077 0.071 Uiso 0.50 1 calc PR C 2
H16D H 0.4685 0.2437 0.0146 0.071 Uiso 0.50 1 calc PR C 2
C17' C 0.5589(12) 0.3843(9) 0.0481(6) 0.131(7) Uani 0.50 1 d PD C 2
H17D H 0.5131 0.4124 0.0740 0.196 Uiso 0.50 1 calc PR C 2
H17E H 0.5578 0.4406 0.0141 0.196 Uiso 0.50 1 calc PR C 2
H17F H 0.6206 0.3856 0.0698 0.196 Uiso 0.50 1 calc PR C 2
C18 C 0.5060(2) -0.0830(3) 0.14553(14) 0.0363(7) Uani 1 1 d . . .
H18A H 0.4479 -0.0880 0.1189 0.044 Uiso 1 1 calc R C .
H18B H 0.5580 -0.0918 0.1209 0.044 Uiso 1 1 calc R . .
C19 C 0.5089(3) -0.1954(3) 0.18894(15) 0.0408(8) Uani 1 1 d . C .
H19A H 0.5703 -0.1990 0.2121 0.049 Uiso 1 1 calc R . .
H19B H 0.4614 -0.1837 0.2168 0.049 Uiso 1 1 calc R . .
C20 C 0.4906(3) -0.3203(3) 0.15475(17) 0.0484(9) Uani 1 1 d . . .
H20A H 0.5373 -0.3305 0.1263 0.058 Uiso 1 1 calc R C .
H20B H 0.4288 -0.3168 0.1322 0.058 Uiso 1 1 calc R . .
C21 C 0.4950(4) -0.4357(4) 0.1969(2) 0.0606(11) Uani 1 1 d . C .
H21A H 0.5538 -0.4349 0.2220 0.091 Uiso 1 1 calc R . .
H21B H 0.4904 -0.5131 0.1736 0.091 Uiso 1 1 calc R . .
H21C H 0.4436 -0.4317 0.2216 0.091 Uiso 1 1 calc R . .
C22 C 0.2861(4) 0.4546(4) 0.0984(2) 0.0714(14) Uani 1 1 d . . .
H22A H 0.3004 0.4109 0.1360 0.107 Uiso 1 1 calc R . .
H22B H 0.2420 0.5224 0.1034 0.107 Uiso 1 1 calc R . .
H22C H 0.3430 0.4897 0.0854 0.107 Uiso 1 1 calc R . .
C23 C 0.2440(3) 0.3629(3) 0.05266(17) 0.0428(8) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.0000 0.0000 0.02186(11) Uani 1 2 d S . .
Mo1 Mo 0.165198(18) 0.06934(2) -0.094081(11) 0.02694(8) Uani 1 1 d . . .
Mo2 Mo 0.215650(17) -0.12772(2) 0.029336(11) 0.02758(8) Uani 1 1 d . . .
Mo3 Mo 0.049442(18) -0.18839(2) 0.117647(11) 0.02917(8) Uani 1 1 d . . .
N1 N 0.51175(19) 0.0501(3) 0.17466(12) 0.0350(6) Uani 1 1 d . C .
O1 O 0.08615(14) 0.21473(19) -0.09489(10) 0.0305(4) Uani 1 1 d . . .
O2 O 0.15426(18) 0.0156(2) -0.16638(10) 0.0421(6) Uani 1 1 d . . .
O3 O 0.27514(16) 0.1331(2) -0.08468(11) 0.0416(5) Uani 1 1 d . . .
O4 O 0.19062(15) -0.11959(18) -0.06509(9) 0.0294(4) Uani 1 1 d . . .
O5 O 0.15623(14) 0.05454(18) 0.00160(9) 0.0252(4) Uani 1 1 d D . .
H5 H 0.1820 0.1142 0.0199 0.038 Uiso 1 1 d RD . .
O6 O 0.32548(16) -0.0632(2) 0.04143(11) 0.0406(5) Uani 1 1 d . . .
O7 O 0.23425(17) -0.2888(2) 0.02255(12) 0.0433(6) Uani 1 1 d . . .
O8 O 0.16970(15) -0.1090(2) 0.10485(9) 0.0323(5) Uani 1 1 d . . .
O9 O 0.05690(13) -0.16989(18) 0.01522(9) 0.0242(4) Uani 1 1 d . . .
O10 O 0.07918(18) -0.3467(2) 0.11686(12) 0.0456(6) Uani 1 1 d . . .
O11 O 0.04847(17) -0.1482(2) 0.19114(10) 0.0432(6) Uani 1 1 d . . .
O12 O -0.01369(14) 0.00483(18) 0.08692(8) 0.0239(4) Uani 1 1 d . . .
O14 O 0.2385(2) 0.2494(2) 0.06423(13) 0.0571(7) Uani 1 1 d . . .
O15 O 0.2117(4) 0.4165(4) -0.00118(19) 0.0994(14) Uani 1 1 d . . .
H15 H 0.1785 0.3647 -0.0211 0.149 Uiso 1 1 calc R . .
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'
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'
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
O9 C1 C4 112.7(2) 3 .
O9 C1 H1A 109.0 3 .
C4 C1 H1A 109.0 . .
O9 C1 H1B 109.1 3 .
C4 C1 H1B 109.0 . .
H1A C1 H1B 107.8 . .
O4 C2 C4 113.2(2) 3 .
O4 C2 H2A 108.9 3 .
C4 C2 H2A 108.9 . .
O4 C2 H2B 108.9 3 .
C4 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
O12 C3 C4 112.5(2) . .
O12 C3 H3A 109.1 . .
C4 C3 H3A 109.1 . .
O12 C3 H3B 109.1 . .
C4 C3 H3B 109.1 . .
H3A C3 H3B 107.8 . .
C2 C4 C5 109.2(3) . .
C2 C4 C1 112.6(3) . .
C5 C4 C1 106.9(4) . .
C2 C4 C3 112.1(3) . .
C5 C4 C3 103.9(4) . .
C1 C4 C3 111.7(2) . .
C2 C4 C5' 98.1(9) . .
C5 C4 C5' 12.6(10) . .
C1 C4 C5' 107.1(16) . .
C3 C4 C5' 114.6(13) . .
O13 C5 C4 109.6(6) . .
O13 C5 H5A 109.8 . .
C4 C5 H5A 109.8 . .
O13 C5 H5B 109.8 . .
C4 C5 H5B 109.8 . .
H5A C5 H5B 108.2 . .
O13' C5' C4 106(2) . .
O13' C5' H5'1 110.5 . .
C4 C5' H5'1 110.5 . .
O13' C5' H5'2 110.5 . .
C4 C5' H5'2 110.5 . .
H5'1 C5' H5'2 108.7 . .
C5' O13' H13' 109.5 . .
C7 C6 N1 115.3(3) . .
C7 C6 H6A 108.4 . .
N1 C6 H6A 108.4 . .
C7 C6 H6B 108.4 . .
N1 C6 H6B 108.4 . .
H6A C6 H6B 107.5 . .
C6 C7 C8 110.7(3) . .
C6 C7 H7A 109.5 . .
C8 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
C9 C8 C7 113.5(3) . .
C9 C8 H8A 108.9 . .
C7 C8 H8A 108.9 . .
C9 C8 H8B 108.9 . .
C7 C8 H8B 108.9 . .
H8A C8 H8B 107.7 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N1 C10 C11 116.3(3) . .
N1 C10 H10A 108.2 . .
C11 C10 H10A 108.2 . .
N1 C10 H10B 108.2 . .
C11 C10 H10B 108.2 . .
H10A C10 H10B 107.4 . .
C10 C11 C12 110.1(4) . .
C10 C11 H11A 109.6 . .
C12 C11 H11A 109.6 . .
C10 C11 H11B 109.6 . .
C12 C11 H11B 109.6 . .
H11A C11 H11B 108.2 . .
C13 C12 C11 113.7(4) . .
C13 C12 H12A 108.8 . .
C11 C12 H12A 108.8 . .
C13 C12 H12B 108.8 . .
C11 C12 H12B 108.8 . .
H12A C12 H12B 107.7 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 N1 116.5(3) . .
C15 C14 H14A 108.2 . .
N1 C14 H14A 108.2 . .
C15 C14 H14B 108.2 . .
N1 C14 H14B 108.2 . .
H14A C14 H14B 107.3 . .
C14 C15 C16 105.2(7) . .
C14 C15 H15A 110.7 . .
C16 C15 H15A 110.7 . .
C14 C15 H15B 110.7 . .
C16 C15 H15B 110.7 . .
H15A C15 H15B 108.8 . .
C17 C16 C15 99.0(13) . .
C17 C16 H16A 112.0 . .
C15 C16 H16A 112.0 . .
C17 C16 H16B 112.0 . .
C15 C16 H16B 112.0 . .
H16A C16 H16B 109.7 . .
C17' C16' H16C 109.6 . .
C17' C16' H16D 109.6 . .
H16C C16' H16D 108.1 . .
C16' C17' H17D 109.5 . .
C16' C17' H17E 109.5 . .
H17D C17' H17E 109.5 . .
C16' C17' H17F 109.5 . .
H17D C17' H17F 109.5 . .
H17E C17' H17F 109.5 . .
C19 C18 N1 115.6(3) . .
C19 C18 H18A 108.4 . .
N1 C18 H18A 108.4 . .
C19 C18 H18B 108.4 . .
N1 C18 H18B 108.4 . .
H18A C18 H18B 107.4 . .
C20 C19 C18 110.5(3) . .
C20 C19 H19A 109.6 . .
C18 C19 H19A 109.6 . .
C20 C19 H19B 109.6 . .
C18 C19 H19B 109.6 . .
H19A C19 H19B 108.1 . .
C19 C20 C21 111.9(3) . .
C19 C20 H20A 109.2 . .
C21 C20 H20A 109.2 . .
C19 C20 H20B 109.2 . .
C21 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C23 C22 H22A 109.5 . .
C23 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C23 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
O14 C23 O15 124.3(4) . .
O14 C23 C22 120.8(4) . .
O15 C23 C22 114.9(3) . .
O9 Cu1 O9 180.00(17) . 3
O9 Cu1 O12 86.12(8) . .
O9 Cu1 O12 93.88(8) 3 .
O9 Cu1 O12 93.88(8) . 3
O9 Cu1 O12 86.12(8) 3 3
O12 Cu1 O12 180.00(11) . 3
O9 Cu1 O5 99.25(7) . 3
O9 Cu1 O5 80.75(7) 3 3
O12 Cu1 O5 80.25(8) . 3
O12 Cu1 O5 99.75(8) 3 3
O9 Cu1 O5 80.75(7) . .
O9 Cu1 O5 99.25(7) 3 .
O12 Cu1 O5 99.75(8) . .
O12 Cu1 O5 80.25(8) 3 .
O5 Cu1 O5 180.00(2) 3 .
O3 Mo1 O2 104.07(12) . .
O3 Mo1 O1 103.13(11) . .
O2 Mo1 O1 104.97(11) . .
O3 Mo1 O4 101.71(10) . .
O2 Mo1 O4 88.80(10) . .
O1 Mo1 O4 147.52(8) . .
O3 Mo1 O5 92.90(10) . .
O2 Mo1 O5 155.04(10) . .
O1 Mo1 O5 88.45(8) . .
O4 Mo1 O5 69.66(7) . .
O3 Mo1 O12 168.36(10) . 3
O2 Mo1 O12 87.56(10) . 3
O1 Mo1 O12 73.21(8) . 3
O4 Mo1 O12 78.27(8) . 3
O5 Mo1 O12 76.10(8) . 3
O6 Mo2 O7 104.81(12) . .
O6 Mo2 O8 102.30(11) . .
O7 Mo2 O8 104.63(11) . .
O6 Mo2 O4 101.79(10) . .
O7 Mo2 O4 87.89(10) . .
O8 Mo2 O4 148.84(9) . .
O6 Mo2 O5 91.38(10) . .
O7 Mo2 O5 154.79(10) . .
O8 Mo2 O5 90.24(8) . .
O4 Mo2 O5 69.70(7) . .
O6 Mo2 O9 167.59(9) . .
O7 Mo2 O9 87.59(10) . .
O8 Mo2 O9 73.56(8) . .
O4 Mo2 O9 78.70(8) . .
O5 Mo2 O9 77.08(7) . .
O11 Mo3 O10 105.99(12) . .
O11 Mo3 O8 97.41(11) . .
O10 Mo3 O8 100.86(10) . .
O11 Mo3 O1 100.51(11) . 3
O10 Mo3 O1 95.73(11) . 3
O8 Mo3 O1 151.14(9) . 3
O11 Mo3 O12 91.80(10) . .
O10 Mo3 O12 160.41(10) . .
O8 Mo3 O12 84.54(8) . .
O1 Mo3 O12 72.51(8) 3 .
O11 Mo3 O9 160.76(10) . .
O10 Mo3 O9 92.00(10) . .
O8 Mo3 O9 72.00(8) . .
O1 Mo3 O9 84.06(8) 3 .
O12 Mo3 O9 71.60(7) . .
C10 N1 C14 112.8(3) . .
C10 N1 C6 109.3(3) . .
C14 N1 C6 107.9(2) . .
C10 N1 C18 107.4(2) . .
C14 N1 C18 108.4(3) . .
C6 N1 C18 111.1(2) . .
Mo1 O1 Mo3 117.30(10) . 3
C2 O4 Mo1 120.53(19) 3 .
C2 O4 Mo2 120.68(18) 3 .
Mo1 O4 Mo2 110.74(9) . .
Mo2 O5 Mo1 106.76(8) . .
Mo2 O5 Cu1 97.91(7) . .
Mo1 O5 Cu1 98.95(8) . .
Mo2 O5 H5 112.9 . .
Mo1 O5 H5 111.9 . .
Cu1 O5 H5 126.0 . .
Mo2 O8 Mo3 118.48(11) . .
C1 O9 Cu1 115.16(17) 3 .
C1 O9 Mo2 119.76(16) 3 .
Cu1 O9 Mo2 103.52(8) . .
C1 O9 Mo3 122.10(16) 3 .
Cu1 O9 Mo3 100.83(8) . .
Mo2 O9 Mo3 91.26(8) . .
C3 O12 Cu1 115.40(16) . .
C3 O12 Mo3 121.55(17) . .
Cu1 O12 Mo3 101.45(8) . .
C3 O12 Mo1 118.89(16) . 3
Cu1 O12 Mo1 104.13(9) . 3
Mo3 O12 Mo1 91.43(7) . 3
C23 O15 H15 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O9 1.438(3) 3
C1 C4 1.542(4) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 O4 1.449(4) 3
C2 C4 1.527(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 O12 1.440(3) .
C3 C4 1.542(4) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.536(7) .
C4 C5' 1.61(4) .
C5 O13 1.428(8) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
O13 H13 0.8200 .
C5' O13' 1.407(19) .
C5' H5'1 0.9700 .
C5' H5'2 0.9700 .
O13' H13' 0.8200 .
C6 C7 1.520(5) .
C6 N1 1.533(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.520(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.516(6) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 N1 1.513(4) .
C10 C11 1.517(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.530(6) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.489(8) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C15 1.516(5) .
C14 N1 1.516(4) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.543(15) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C17 1.462(16) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C16' C17' 1.503(14) .
C16' H16C 0.9700 .
C16' H16D 0.9700 .
C17' H17D 0.9600 .
C17' H17E 0.9600 .
C17' H17F 0.9600 .
C18 C19 1.521(4) .
C18 N1 1.533(4) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.520(5) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 C21 1.526(5) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 C23 1.481(5) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 O14 1.217(4) .
C23 O15 1.364(5) .
Cu1 O9 1.9652(19) .
Cu1 O9 1.9652(19) 3
Cu1 O12 1.9709(18) .
Cu1 O12 1.9709(18) 3
Cu1 O5 2.292(2) 3
Cu1 O5 2.292(2) .
Mo1 O3 1.694(2) .
Mo1 O2 1.702(2) .
Mo1 O1 1.888(2) .
Mo1 O4 2.096(2) .
Mo1 O5 2.159(2) .
Mo1 O12 2.3113(19) 3
Mo2 O6 1.698(2) .
Mo2 O7 1.712(2) .
Mo2 O8 1.879(2) .
Mo2 O4 2.105(2) .
Mo2 O5 2.148(2) .
Mo2 O9 2.292(2) .
Mo3 O11 1.695(2) .
Mo3 O10 1.707(2) .
Mo3 O8 1.948(2) .
Mo3 O1 1.965(2) 3
Mo3 O12 2.286(2) .
Mo3 O9 2.309(2) .
O1 Mo3 1.965(2) 3
O4 C2 1.449(4) 3
O5 H5 0.8118 .
O9 C1 1.438(3) 3
O12 Mo1 2.3113(19) 3
O15 H15 0.8200 .
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_4
O4 C2 C4 C5 -178.2(4) 3 .
O4 C2 C4 C1 63.3(3) 3 .
O4 C2 C4 C3 -63.7(3) 3 .
O4 C2 C4 C5' 175.6(16) 3 .
O9 C1 C4 C2 -60.3(3) 3 .
O9 C1 C4 C5 179.9(4) 3 .
O9 C1 C4 C3 66.8(3) 3 .
O9 C1 C4 C5' -167.0(9) 3 .
O12 C3 C4 C2 61.0(3) . .
O12 C3 C4 C5 178.8(4) . .
O12 C3 C4 C1 -66.3(3) . .
O12 C3 C4 C5' 171.7(14) . .
C2 C4 C5 O13 -53.0(6) . .
C1 C4 C5 O13 69.0(5) . .
C3 C4 C5 O13 -172.7(4) . .
C5' C4 C5 O13 -24(8) . .
C2 C4 C5' O13' 171(2) . .
C5 C4 C5' O13' 19(6) . .
C1 C4 C5' O13' -73(3) . .
C3 C4 C5' O13' 52(3) . .
N1 C6 C7 C8 -176.5(3) . .
C6 C7 C8 C9 76.6(4) . .
N1 C10 C11 C12 -179.5(4) . .
C10 C11 C12 C13 -63.4(5) . .
N1 C14 C15 C16 -161.7(9) . .
C14 C15 C16 C17 -82.9(11) . .
N1 C18 C19 C20 173.1(3) . .
C18 C19 C20 C21 178.8(3) . .
C11 C10 N1 C14 56.4(5) . .
C11 C10 N1 C6 -63.6(4) . .
C11 C10 N1 C18 175.8(4) . .
C15 C14 N1 C10 57.7(5) . .
C15 C14 N1 C6 178.5(4) . .
C15 C14 N1 C18 -61.1(5) . .
C7 C6 N1 C10 -169.3(3) . .
C7 C6 N1 C14 67.7(4) . .
C7 C6 N1 C18 -51.0(4) . .
C19 C18 N1 C10 65.5(4) . .
C19 C18 N1 C14 -172.3(3) . .
C19 C18 N1 C6 -53.9(4) . .
O3 Mo1 O1 Mo3 170.60(12) . 3
O2 Mo1 O1 Mo3 61.89(14) . 3
O4 Mo1 O1 Mo3 -50.4(2) . 3
O5 Mo1 O1 Mo3 -96.78(12) . 3
O12 Mo1 O1 Mo3 -20.83(10) 3 3
O3 Mo1 O4 C2 -136.4(2) . 3
O2 Mo1 O4 C2 -32.2(2) . 3
O1 Mo1 O4 C2 84.4(2) . 3
O5 Mo1 O4 C2 134.9(2) . 3
O12 Mo1 O4 C2 55.51(19) 3 3
O3 Mo1 O4 Mo2 74.68(12) . .
O2 Mo1 O4 Mo2 178.80(11) . .
O1 Mo1 O4 Mo2 -64.6(2) . .
O5 Mo1 O4 Mo2 -14.08(8) . .
O12 Mo1 O4 Mo2 -93.44(10) 3 .
O6 Mo2 O4 C2 138.2(2) . 3
O7 Mo2 O4 C2 33.5(2) . 3
O8 Mo2 O4 C2 -81.8(3) . 3
O5 Mo2 O4 C2 -134.8(2) . 3
O9 Mo2 O4 C2 -54.5(2) . 3
O6 Mo2 O4 Mo1 -72.94(12) . .
O7 Mo2 O4 Mo1 -177.63(12) . .
O8 Mo2 O4 Mo1 67.05(19) . .
O5 Mo2 O4 Mo1 14.14(8) . .
O9 Mo2 O4 Mo1 94.40(10) . .
O6 Mo2 O5 Mo1 88.66(11) . .
O7 Mo2 O5 Mo1 -42.0(3) . .
O8 Mo2 O5 Mo1 -169.02(9) . .
O4 Mo2 O5 Mo1 -13.40(8) . .
O9 Mo2 O5 Mo1 -95.96(9) . .
O6 Mo2 O5 Cu1 -169.46(10) . .
O7 Mo2 O5 Cu1 59.9(2) . .
O8 Mo2 O5 Cu1 -67.15(9) . .
O4 Mo2 O5 Cu1 88.48(9) . .
O9 Mo2 O5 Cu1 5.92(6) . .
O3 Mo1 O5 Mo2 -87.95(11) . .
O2 Mo1 O5 Mo2 45.3(3) . .
O1 Mo1 O5 Mo2 168.98(9) . .
O4 Mo1 O5 Mo2 13.46(8) . .
O12 Mo1 O5 Mo2 95.90(9) 3 .
O3 Mo1 O5 Cu1 170.92(10) . .
O2 Mo1 O5 Cu1 -55.8(3) . .
O1 Mo1 O5 Cu1 67.85(8) . .
O4 Mo1 O5 Cu1 -87.66(8) . .
O12 Mo1 O5 Cu1 -5.22(6) 3 .
O9 Cu1 O5 Mo2 -6.82(7) . .
O9 Cu1 O5 Mo2 173.18(7) 3 .
O12 Cu1 O5 Mo2 77.58(8) . .
O12 Cu1 O5 Mo2 -102.42(8) 3 .
O5 Cu1 O5 Mo2 -126(56) 3 .
O9 Cu1 O5 Mo1 101.64(8) . .
O9 Cu1 O5 Mo1 -78.36(8) 3 .
O12 Cu1 O5 Mo1 -173.96(7) . .
O12 Cu1 O5 Mo1 6.04(7) 3 .
O5 Cu1 O5 Mo1 -18(56) 3 .
O6 Mo2 O8 Mo3 -172.58(12) . .
O7 Mo2 O8 Mo3 -63.47(15) . .
O4 Mo2 O8 Mo3 47.5(2) . .
O5 Mo2 O8 Mo3 95.95(12) . .
O9 Mo2 O8 Mo3 19.51(10) . .
O11 Mo3 O8 Mo2 176.96(13) . .
O10 Mo3 O8 Mo2 69.03(15) . .
O1 Mo3 O8 Mo2 -54.9(2) 3 .
O12 Mo3 O8 Mo2 -91.93(12) . .
O9 Mo3 O8 Mo2 -19.53(10) . .
O9 Cu1 O9 C1 -45(77) 3 3
O12 Cu1 O9 C1 133.35(18) . 3
O12 Cu1 O9 C1 -46.65(18) 3 3
O5 Cu1 O9 C1 53.90(18) 3 3
O5 Cu1 O9 C1 -126.10(18) . 3
O9 Cu1 O9 Mo2 88(77) 3 .
O12 Cu1 O9 Mo2 -94.04(9) . .
O12 Cu1 O9 Mo2 85.96(9) 3 .
O5 Cu1 O9 Mo2 -173.49(7) 3 .
O5 Cu1 O9 Mo2 6.51(7) . .
O9 Cu1 O9 Mo3 -178(77) 3 .
O12 Cu1 O9 Mo3 -0.09(8) . .
O12 Cu1 O9 Mo3 179.91(8) 3 .
O5 Cu1 O9 Mo3 -79.54(8) 3 .
O5 Cu1 O9 Mo3 100.46(8) . .
O6 Mo2 O9 C1 144.9(4) . 3
O7 Mo2 O9 C1 -37.0(2) . 3
O8 Mo2 O9 C1 -143.0(2) . 3
O4 Mo2 O9 C1 51.33(18) . 3
O5 Mo2 O9 C1 122.84(19) . 3
O6 Mo2 O9 Cu1 15.0(5) . .
O7 Mo2 O9 Cu1 -166.87(11) . .
O8 Mo2 O9 Cu1 87.11(10) . .
O4 Mo2 O9 Cu1 -78.54(8) . .
O5 Mo2 O9 Cu1 -7.03(7) . .
O6 Mo2 O9 Mo3 -86.5(4) . .
O7 Mo2 O9 Mo3 91.68(10) . .
O8 Mo2 O9 Mo3 -14.35(8) . .
O4 Mo2 O9 Mo3 180.00(8) . .
O5 Mo2 O9 Mo3 -108.49(7) . .
O11 Mo3 O9 C1 -160.5(3) . 3
O10 Mo3 O9 C1 40.0(2) . 3
O8 Mo3 O9 C1 140.8(2) . 3
O1 Mo3 O9 C1 -55.5(2) 3 3
O12 Mo3 O9 C1 -129.0(2) . 3
O11 Mo3 O9 Cu1 -31.4(3) . .
O10 Mo3 O9 Cu1 169.15(11) . .
O8 Mo3 O9 Cu1 -90.08(10) . .
O1 Mo3 O9 Cu1 73.59(9) 3 .
O12 Mo3 O9 Cu1 0.08(7) . .
O11 Mo3 O9 Mo2 72.7(3) . .
O10 Mo3 O9 Mo2 -86.83(10) . .
O8 Mo3 O9 Mo2 13.94(8) . .
O1 Mo3 O9 Mo2 177.62(8) 3 .
O12 Mo3 O9 Mo2 104.10(8) . .
C4 C3 O12 Cu1 60.8(3) . .
C4 C3 O12 Mo3 -175.84(16) . .
C4 C3 O12 Mo1 -64.0(3) . 3
O9 Cu1 O12 C3 133.50(19) . .
O9 Cu1 O12 C3 -46.50(19) 3 .
O12 Cu1 O12 C3 151.9(6) 3 .
O5 Cu1 O12 C3 -126.41(19) 3 .
O5 Cu1 O12 C3 53.59(19) . .
O9 Cu1 O12 Mo3 0.09(8) . .
O9 Cu1 O12 Mo3 -179.91(8) 3 .
O12 Cu1 O12 Mo3 18.5(3) 3 .
O5 Cu1 O12 Mo3 100.17(8) 3 .
O5 Cu1 O12 Mo3 -79.83(8) . .
O9 Cu1 O12 Mo1 -94.34(8) . 3
O9 Cu1 O12 Mo1 85.66(8) 3 3
O12 Cu1 O12 Mo1 -75.9(3) 3 3
O5 Cu1 O12 Mo1 5.74(7) 3 3
O5 Cu1 O12 Mo1 -174.26(7) . 3
O11 Mo3 O12 C3 40.4(2) . .
O10 Mo3 O12 C3 -164.1(3) . .
O8 Mo3 O12 C3 -56.90(19) . .
O1 Mo3 O12 C3 140.8(2) 3 .
O9 Mo3 O12 C3 -129.7(2) . .
O11 Mo3 O12 Cu1 170.02(10) . .
O10 Mo3 O12 Cu1 -34.5(3) . .
O8 Mo3 O12 Cu1 72.74(9) . .
O1 Mo3 O12 Cu1 -89.53(10) 3 .
O9 Mo3 O12 Cu1 -0.08(7) . .
O11 Mo3 O12 Mo1 -85.25(10) . 3
O10 Mo3 O12 Mo1 70.3(3) . 3
O8 Mo3 O12 Mo1 177.47(8) . 3
O1 Mo3 O12 Mo1 15.20(7) 3 3
O9 Mo3 O12 Mo1 104.65(8) . 3
