#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:07:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180466 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/35/7213581.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_7213581
loop_
_publ_author_name
'Smith, Tiffany M.'
'Perkins, Kathryn'
'Symester, Diona'
'Freund, Steve R.'
'Vargas, Jose'
'Spinu, Leonard'
'Zubieta, Jon'
_publ_section_title
;
 Solid state coordination chemistry of oxomolybdenum--organodiphosphonate
 materials: consequences of introducing xylyldiphosphonate components
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              191
_journal_paper_doi               10.1039/c3ce41728j
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C32 H32 Cu2 Mo5 N4 O25 P2, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Cu2 Mo5 N4 O29 P2'
_chemical_formula_weight         1613.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 118.357(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4404(14)
_cell_length_b                   21.237(2)
_cell_length_c                   18.1894(14)
_cell_measurement_reflns_used    6598
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      33.0412
_cell_measurement_theta_min      1.6906
_cell_volume                     4568.9(8)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0355
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            86173
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.165
_diffrn_reflns_theta_min         1.722
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_density_meas      2.36(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.127
_refine_diff_density_max         1.875
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         17963
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0350
_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/[σ²(Fo²)+(0.0198P)²+21.3187P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14688
_reflns_number_total             17963
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce41728j.txt
_cod_data_source_block           compound6
_cod_database_code               7213581
#BEGIN Tags that were not found in dictionaries:
_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   0.501
_shelx_estimated_absorpt_t_max   0.749
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo1 Mo 1.25011(2) 0.71780(2) 0.88020(2) 0.00818(4) Uani 1 1 d . .
Mo2 Mo 1.32390(2) 0.63808(2) 0.75412(2) 0.00868(4) Uani 1 1 d . .
Mo3 Mo 1.10166(2) 0.55259(2) 0.61561(2) 0.00798(4) Uani 1 1 d . .
Mo4 Mo 0.87314(2) 0.59728(2) 0.63040(2) 0.00813(4) Uani 1 1 d . .
Mo5 Mo 0.98604(2) 0.67466(2) 0.83768(2) 0.00787(4) Uani 1 1 d . .
Cu1 Cu 0.82358(3) 0.81329(2) 0.82056(2) 0.01037(6) Uani 1 1 d . .
Cu2 Cu 0.73862(3) 0.45654(2) 0.64505(2) 0.01020(6) Uani 1 1 d . .
P1 P 1.05749(6) 0.70785(3) 0.67279(4) 0.00787(11) Uani 1 1 d . .
P2 P 0.85937(6) 1.06728(3) 0.68598(4) 0.00746(11) Uani 1 1 d . .
O1 O 1.13779(16) 0.69560(10) 0.91600(12) 0.0089(3) Uani 1 1 d . .
O2 O 1.23915(18) 0.79772(10) 0.88380(14) 0.0127(4) Uani 1 1 d . .
O3 O 1.36770(17) 0.70083(10) 0.97281(13) 0.0122(4) Uani 1 1 d . .
O4 O 1.30727(17) 0.71478(10) 0.80218(13) 0.0106(4) Uani 1 1 d . .
O5 O 1.08426(16) 0.70744(10) 0.76547(12) 0.0097(3) Uani 1 1 d . .
O6 O 1.45059(17) 0.61062(11) 0.83144(14) 0.0141(4) Uani 1 1 d . .
O7 O 1.35760(18) 0.66741(11) 0.68094(14) 0.0152(4) Uani 1 1 d . .
O8 O 1.25296(16) 0.56045(10) 0.70544(12) 0.0098(3) Uani 1 1 d . .
O9 O 1.13679(16) 0.66277(10) 0.65799(12) 0.0092(3) Uani 1 1 d . .
O10 O 1.12548(17) 0.56748(10) 0.53275(13) 0.0118(4) Uani 1 1 d . .
O11 O 1.08975(17) 0.47286(10) 0.61600(13) 0.0123(4) Uani 1 1 d . .
O12 O 0.94230(16) 0.57670(10) 0.56471(12) 0.0097(3) Uani 1 1 d . .
O13 O 0.84219(17) 0.52125(10) 0.65185(13) 0.0123(4) Uani 1 1 d . .
O14 O 0.74263(17) 0.62150(11) 0.55812(13) 0.0135(4) Uani 1 1 d . .
O15 O 0.93416(16) 0.69050(10) 0.61860(12) 0.0097(3) Uani 1 1 d . .
O16 O 0.88748(16) 0.63637(10) 0.73122(12) 0.0095(3) Uani 1 1 d . .
O17 O 0.93417(18) 0.64604(11) 0.89938(13) 0.0131(4) Uani 1 1 d . .
O18 O 0.92557(17) 0.75035(10) 0.81644(13) 0.0111(4) Uani 1 1 d . .
O19 O 0.9422(2) 0.84512(13) 0.92713(16) 0.0225(5) Uani 1 1 d D .
H19C H 0.919(4) 0.824(2) 0.953(3) 0.027 Uiso 1 1 d D U
H19D H 1.008(2) 0.830(2) 0.947(3) 0.027 Uiso 1 1 d D U
O20 O 0.7712(2) 0.75436(14) 0.90043(19) 0.0259(5) Uani 1 1 d D .
H20C H 0.732(4) 0.737(2) 0.8539(19) 0.031 Uiso 1 1 d D U
H20D H 0.759(4) 0.7156(10) 0.903(3) 0.031 Uiso 1 1 d D U
O21 O 0.92830(16) 1.08313(10) 0.64258(12) 0.0092(3) Uani 1 1 d . .
O22 O 0.93884(16) 1.06640(10) 0.78116(12) 0.0087(3) Uani 1 1 d . .
O23 O 0.76055(16) 1.11392(10) 0.66258(13) 0.0095(3) Uani 1 1 d . .
O24 O 0.74350(19) 0.41630(11) 0.54727(14) 0.0145(4) Uani 1 1 d D .
H24C H 0.783(3) 0.425(2) 0.525(2) 0.017 Uiso 1 1 d D U
H24D H 0.752(4) 0.3780(9) 0.552(3) 0.017 Uiso 1 1 d D U
O25 O 0.5922(2) 0.52392(15) 0.5789(2) 0.0396(8) Uani 1 1 d D .
H25C H 0.602(5) 0.5572(17) 0.605(3) 0.047 Uiso 1 1 d D U
H25D H 0.573(5) 0.517(3) 0.5297(16) 0.047 Uiso 1 1 d D U
O90 O 0.6724(2) 0.86250(17) 0.3564(2) 0.0344(7) Uani 1 1 d D .
H90A H 0.606(2) 0.872(3) 0.348(3) 0.041 Uiso 1 1 d D U
H90B H 0.666(5) 0.871(3) 0.3085(19) 0.041 Uiso 1 1 d D U
O91 O 0.6545(2) 0.87676(15) 0.19520(19) 0.0270(6) Uani 1 1 d D .
H91A H 0.679(4) 0.8439(16) 0.226(3) 0.032 Uiso 1 1 d D U
H91B H 0.608(4) 0.8474(19) 0.167(3) 0.032 Uiso 1 1 d D U
O92 O 0.5231(2) 0.30168(14) 0.40767(17) 0.0228(5) Uani 1 1 d . .
H92A H 0.549(4) 0.276(3) 0.442(3) 0.027 Uiso 1 1 d . U
H92B H 0.561(4) 0.313(2) 0.387(3) 0.027 Uiso 1 1 d . U
O93 O 0.1520(2) 0.69726(12) 0.50521(15) 0.0172(4) Uani 1 1 d D .
H93A H 0.178(3) 0.696(2) 0.5571(12) 0.021 Uiso 1 1 d D U
H93B H 0.160(4) 0.7351(11) 0.496(3) 0.021 Uiso 1 1 d D U
N1 N 0.7126(2) 0.87998(12) 0.81167(16) 0.0119(4) Uani 1 1 d . .
N2 N 0.7327(2) 0.81422(12) 0.69718(16) 0.0122(4) Uani 1 1 d . .
N3 N 0.6314(2) 0.39292(12) 0.64591(15) 0.0110(4) Uani 1 1 d . .
N4 N 0.7799(2) 0.46410(12) 0.76555(15) 0.0112(4) Uani 1 1 d . .
C1 C 0.7042(2) 0.91058(15) 0.87198(19) 0.0149(5) Uani 1 1 d . .
H1 H 0.7524 0.8999 0.9273 0.018 Uiso 1 1 calc R U
C2 C 0.6239(3) 0.95887(15) 0.8544(2) 0.0166(5) Uani 1 1 d . .
H2 H 0.6184 0.9789 0.8978 0.020 Uiso 1 1 calc R U
C3 C 0.5541(3) 0.97617(15) 0.7735(2) 0.0178(6) Uani 1 1 d . .
H3 H 0.5019 1.0084 0.7618 0.021 Uiso 1 1 calc R U
C4 C 0.6413(2) 0.89567(14) 0.73121(18) 0.0113(5) Uani 1 1 d . .
C5 C 0.5617(2) 0.94485(15) 0.7080(2) 0.0145(5) Uani 1 1 d . .
C6 C 0.4951(2) 0.95893(15) 0.6207(2) 0.0169(6) Uani 1 1 d . .
H6 H 0.4432 0.9918 0.6044 0.020 Uiso 1 1 calc R U
C7 C 0.5062(3) 0.92533(16) 0.5611(2) 0.0175(6) Uani 1 1 d . .
H7 H 0.4611 0.9352 0.5050 0.021 Uiso 1 1 calc R U
C8 C 0.5866(2) 0.87490(15) 0.58402(18) 0.0135(5) Uani 1 1 d . .
C9 C 0.6527(2) 0.86044(14) 0.66888(18) 0.0117(5) Uani 1 1 d . .
C10 C 0.7514(2) 0.78235(15) 0.64178(19) 0.0142(5) Uani 1 1 d . .
H10 H 0.8065 0.7511 0.6607 0.017 Uiso 1 1 calc R U
C11 C 0.6903(3) 0.79457(16) 0.55578(19) 0.0164(5) Uani 1 1 d . .
H11 H 0.7060 0.7721 0.5186 0.020 Uiso 1 1 calc R U
C12 C 0.6070(3) 0.84003(16) 0.52659(19) 0.0164(6) Uani 1 1 d . .
H12 H 0.5647 0.8476 0.4696 0.020 Uiso 1 1 calc R U
C13 C 0.5498(2) 0.36202(15) 0.58267(19) 0.0141(5) Uani 1 1 d . .
H13 H 0.5365 0.3706 0.5286 0.017 Uiso 1 1 calc R U
C14 C 0.4832(2) 0.31698(15) 0.5948(2) 0.0171(6) Uani 1 1 d . .
H14 H 0.4249 0.2972 0.5489 0.020 Uiso 1 1 calc R U
C15 C 0.5032(2) 0.30180(15) 0.6738(2) 0.0170(6) Uani 1 1 d . .
H15 H 0.4607 0.2708 0.6820 0.020 Uiso 1 1 calc R U
C16 C 0.5893(2) 0.33385(14) 0.7427(2) 0.0138(5) Uani 1 1 d . .
C17 C 0.6486(2) 0.38027(14) 0.72420(18) 0.0113(5) Uani 1 1 d . .
C18 C 0.7301(2) 0.41882(14) 0.78984(18) 0.0112(5) Uani 1 1 d . .
C19 C 0.6174(3) 0.32380(15) 0.8283(2) 0.0162(5) Uani 1 1 d . .
H19A H 0.5805 0.2922 0.8415 0.019 Uiso 1 1 calc R U
C20 C 0.6967(3) 0.35931(15) 0.8906(2) 0.0161(5) Uani 1 1 d . .
H20A H 0.7143 0.3512 0.9457 0.019 Uiso 1 1 calc R U
C21 C 0.7539(2) 0.40943(15) 0.87249(18) 0.0133(5) Uani 1 1 d . .
C22 C 0.8303(3) 0.45163(15) 0.93252(18) 0.0148(5) Uani 1 1 d . .
H22 H 0.8490 0.4475 0.9885 0.018 Uiso 1 1 calc R U
C23 C 0.8768(3) 0.49905(15) 0.90704(19) 0.0156(5) Uani 1 1 d . .
H23 H 0.9251 0.5282 0.9456 0.019 Uiso 1 1 calc R U
C24 C 0.8514(2) 0.50342(15) 0.82283(18) 0.0135(5) Uani 1 1 d . .
H24 H 0.8857 0.5347 0.8069 0.016 Uiso 1 1 calc R U
C25 C 1.0844(2) 0.78609(13) 0.64805(18) 0.0106(5) Uani 1 1 d . .
H25A H 1.1623 0.7967 0.6864 0.013 Uiso 1 1 calc R U
H25B H 1.0768 0.7853 0.5923 0.013 Uiso 1 1 calc R U
C26 C 1.0096(2) 0.83855(13) 0.65122(17) 0.0096(4) Uani 1 1 d . .
C27 C 0.9309(2) 0.86740(14) 0.57722(18) 0.0118(5) Uani 1 1 d . .
H27 H 0.9239 0.8537 0.5264 0.014 Uiso 1 1 calc R U
C28 C 1.0186(2) 0.86041(14) 0.72660(18) 0.0117(5) Uani 1 1 d . .
H28 H 1.0700 0.8416 0.7765 0.014 Uiso 1 1 calc R U
C29 C 0.8629(2) 0.91633(14) 0.57856(18) 0.0118(5) Uani 1 1 d . .
H29 H 0.8102 0.9345 0.5286 0.014 Uiso 1 1 calc R U
C30 C 0.9518(2) 0.91007(14) 0.72811(18) 0.0121(5) Uani 1 1 d . .
H30 H 0.9599 0.9244 0.7790 0.015 Uiso 1 1 calc R U
C31 C 0.8728(2) 0.93855(13) 0.65403(18) 0.0099(4) Uani 1 1 d . .
C32 C 0.7958(2) 0.99082(13) 0.65348(18) 0.0102(5) Uani 1 1 d . .
H32A H 0.7645 0.9785 0.6896 0.012 Uiso 1 1 calc R U
H32B H 0.7333 0.9945 0.5973 0.012 Uiso 1 1 calc R 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'
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'
P P 0.1023 0.0942 '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
O2 Mo1 O3 103.14(11) . .
O2 Mo1 O4 97.73(10) . .
O3 Mo1 O4 102.40(9) . .
O2 Mo1 O1 97.58(9) . .
O3 Mo1 O1 96.82(9) . .
O4 Mo1 O1 151.93(8) . .
O2 Mo1 O5 93.90(9) . .
O3 Mo1 O5 161.14(9) . .
O4 Mo1 O5 82.94(8) . .
O1 Mo1 O5 72.66(8) . .
O2 Mo1 O23 164.78(9) . 2_746
O3 Mo1 O23 90.63(9) . 2_746
O4 Mo1 O23 72.62(8) . 2_746
O1 Mo1 O23 87.03(8) . 2_746
O5 Mo1 O23 73.55(7) . 2_746
O7 Mo2 O6 103.57(11) . .
O7 Mo2 O8 102.27(10) . .
O6 Mo2 O8 99.80(10) . .
O7 Mo2 O4 100.19(10) . .
O6 Mo2 O4 101.59(10) . .
O8 Mo2 O4 144.19(8) . .
O7 Mo2 O9 85.69(9) . .
O6 Mo2 O9 169.89(9) . .
O8 Mo2 O9 73.91(8) . .
O4 Mo2 O9 80.40(8) . .
O7 Mo2 O23 166.04(9) . 2_746
O6 Mo2 O23 89.58(9) . 2_746
O8 Mo2 O23 79.70(8) . 2_746
O4 Mo2 O23 72.11(8) . 2_746
O9 Mo2 O23 81.57(7) . 2_746
O11 Mo3 O10 104.17(10) . .
O11 Mo3 O8 98.45(9) . .
O10 Mo3 O8 99.66(9) . .
O11 Mo3 O12 100.29(9) . .
O10 Mo3 O12 98.95(9) . .
O8 Mo3 O12 149.38(8) . .
O11 Mo3 O22 93.85(9) . 2_746
O10 Mo3 O22 161.48(9) . 2_746
O8 Mo3 O22 81.60(8) . 2_746
O12 Mo3 O22 73.20(8) . 2_746
O11 Mo3 O9 163.39(9) . .
O10 Mo3 O9 90.68(9) . .
O8 Mo3 O9 71.29(8) . .
O12 Mo3 O9 84.41(8) . .
O22 Mo3 O9 72.11(7) 2_746 .
O14 Mo4 O13 100.60(10) . .
O14 Mo4 O12 102.66(10) . .
O13 Mo4 O12 99.67(10) . .
O14 Mo4 O16 101.83(10) . .
O13 Mo4 O16 96.38(9) . .
O12 Mo4 O16 147.56(8) . .
O14 Mo4 O15 87.00(9) . .
O13 Mo4 O15 172.23(9) . .
O12 Mo4 O15 80.04(8) . .
O16 Mo4 O15 80.33(8) . .
O14 Mo4 O22 173.22(9) . 2_746
O13 Mo4 O22 83.26(8) . 2_746
O12 Mo4 O22 71.06(8) . 2_746
O16 Mo4 O22 83.14(8) . 2_746
O15 Mo4 O22 89.34(7) . 2_746
O17 Mo5 O18 100.44(10) . .
O17 Mo5 O1 102.72(9) . .
O18 Mo5 O1 99.78(9) . .
O17 Mo5 O16 102.21(10) . .
O18 Mo5 O16 98.00(9) . .
O1 Mo5 O16 146.02(8) . .
O17 Mo5 O21 85.57(9) . 2_746
O18 Mo5 O21 173.95(8) . 2_746
O1 Mo5 O21 78.04(8) . 2_746
O16 Mo5 O21 81.26(8) . 2_746
O17 Mo5 O5 171.45(9) . .
O18 Mo5 O5 86.03(8) . .
O1 Mo5 O5 70.42(8) . .
O16 Mo5 O5 82.25(8) . .
O21 Mo5 O5 87.93(7) 2_746 .
O18 Cu1 O19 91.05(10) . .
O18 Cu1 N2 91.71(10) . .
O19 Cu1 N2 153.33(12) . .
O18 Cu1 N1 173.81(10) . .
O19 Cu1 N1 93.47(10) . .
N2 Cu1 N1 82.36(10) . .
O18 Cu1 O20 94.85(10) . .
O19 Cu1 O20 84.87(12) . .
N2 Cu1 O20 121.28(11) . .
N1 Cu1 O20 89.77(10) . .
O13 Cu2 N3 175.35(10) . .
O13 Cu2 N4 93.26(10) . .
N3 Cu2 N4 82.52(10) . .
O13 Cu2 O24 91.96(9) . .
N3 Cu2 O24 92.69(10) . .
N4 Cu2 O24 154.25(10) . .
O13 Cu2 O25 90.13(11) . .
N3 Cu2 O25 89.05(12) . .
N4 Cu2 O25 104.54(12) . .
O24 Cu2 O25 100.65(12) . .
O15 P1 O5 108.86(11) . .
O15 P1 O9 111.51(12) . .
O5 P1 O9 111.27(11) . .
O15 P1 C25 110.38(12) . .
O5 P1 C25 107.86(13) . .
O9 P1 C25 106.89(12) . .
O21 P2 O22 108.60(11) . .
O21 P2 O23 111.89(11) . .
O22 P2 O23 111.28(11) . .
O21 P2 C32 110.01(12) . .
O22 P2 C32 108.99(13) . .
O23 P2 C32 106.02(12) . .
Mo5 O1 Mo1 121.78(10) . .
Mo1 O4 Mo2 122.99(11) . .
P1 O5 Mo1 129.19(11) . .
P1 O5 Mo5 134.74(11) . .
Mo1 O5 Mo5 94.76(7) . .
Mo2 O8 Mo3 124.55(11) . .
P1 O9 Mo2 126.34(11) . .
P1 O9 Mo3 127.04(11) . .
Mo2 O9 Mo3 89.96(7) . .
Mo4 O12 Mo3 121.38(10) . .
Mo4 O13 Cu2 152.30(13) . .
P1 O15 Mo4 119.98(11) . .
Mo5 O16 Mo4 147.36(11) . .
Mo5 O18 Cu1 151.84(13) . .
Cu1 O19 H19C 91(4) . .
Cu1 O19 H19D 119(3) . .
H19C O19 H19D 99(5) . .
Cu1 O20 H20C 81(4) . .
Cu1 O20 H20D 134(4) . .
H20C O20 H20D 64(4) . .
P2 O21 Mo5 120.93(11) . 2_756
P2 O22 Mo3 129.53(11) . 2_756
P2 O22 Mo4 135.20(11) . 2_756
Mo3 O22 Mo4 94.25(7) 2_756 2_756
P2 O23 Mo1 127.56(11) . 2_756
P2 O23 Mo2 125.42(11) . 2_756
Mo1 O23 Mo2 92.12(7) 2_756 2_756
Cu2 O24 H24C 129(3) . .
Cu2 O24 H24D 113(3) . .
H24C O24 H24D 101(4) . .
Cu2 O25 H25C 112(4) . .
Cu2 O25 H25D 102(4) . .
H25C O25 H25D 132(6) . .
H90A O90 H90B 100(5) . .
H91A O91 H91B 75(4) . .
H92A O92 H92B 116(5) . .
H93A O93 H93B 104(4) . .
C1 N1 C4 118.6(3) . .
C1 N1 Cu1 129.2(2) . .
C4 N1 Cu1 112.18(19) . .
C10 N2 C9 118.5(3) . .
C10 N2 Cu1 128.0(2) . .
C9 N2 Cu1 112.7(2) . .
C13 N3 C17 118.1(3) . .
C13 N3 Cu2 129.5(2) . .
C17 N3 Cu2 112.41(19) . .
C24 N4 C18 118.4(3) . .
C24 N4 Cu2 129.3(2) . .
C18 N4 Cu2 112.15(19) . .
N1 C1 C2 121.7(3) . .
N1 C1 H1 119.2 . .
C2 C1 H1 119.2 . .
C3 C2 C1 120.0(3) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C5 119.6(3) . .
C2 C3 H3 120.2 . .
C5 C3 H3 120.2 . .
N1 C4 C5 123.5(3) . .
N1 C4 C9 116.2(3) . .
C5 C4 C9 120.3(3) . .
C4 C5 C3 116.5(3) . .
C4 C5 C6 118.1(3) . .
C3 C5 C6 125.4(3) . .
C7 C6 C5 121.6(3) . .
C7 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
C6 C7 C8 120.7(3) . .
C6 C7 H7 119.6 . .
C8 C7 H7 119.6 . .
C9 C8 C12 117.2(3) . .
C9 C8 C7 118.6(3) . .
C12 C8 C7 124.2(3) . .
N2 C9 C8 123.2(3) . .
N2 C9 C4 116.2(3) . .
C8 C9 C4 120.6(3) . .
N2 C10 C11 121.9(3) . .
N2 C10 H10 119.0 . .
C11 C10 H10 119.0 . .
C12 C11 C10 119.8(3) . .
C12 C11 H11 120.1 . .
C10 C11 H11 120.1 . .
C11 C12 C8 119.4(3) . .
C11 C12 H12 120.3 . .
C8 C12 H12 120.3 . .
N3 C13 C14 122.0(3) . .
N3 C13 H13 119.0 . .
C14 C13 H13 119.0 . .
C15 C14 C13 120.3(3) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C14 C15 C16 119.2(3) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
C17 C16 C15 116.4(3) . .
C17 C16 C19 118.5(3) . .
C15 C16 C19 125.1(3) . .
N3 C17 C16 123.8(3) . .
N3 C17 C18 116.3(2) . .
C16 C17 C18 119.8(3) . .
N4 C18 C21 123.7(3) . .
N4 C18 C17 115.6(3) . .
C21 C18 C17 120.7(3) . .
C20 C19 C16 121.5(3) . .
C20 C19 H19A 119.3 . .
C16 C19 H19A 119.3 . .
C19 C20 C21 120.8(3) . .
C19 C20 H20A 119.6 . .
C21 C20 H20A 119.6 . .
C18 C21 C22 117.0(3) . .
C18 C21 C20 118.6(3) . .
C22 C21 C20 124.4(3) . .
C23 C22 C21 119.0(3) . .
C23 C22 H22 120.5 . .
C21 C22 H22 120.5 . .
C22 C23 C24 120.1(3) . .
C22 C23 H23 120.0 . .
C24 C23 H23 120.0 . .
N4 C24 C23 121.7(3) . .
N4 C24 H24 119.2 . .
C23 C24 H24 119.2 . .
C26 C25 P1 116.88(19) . .
C26 C25 H25A 108.1 . .
P1 C25 H25A 108.1 . .
C26 C25 H25B 108.1 . .
P1 C25 H25B 108.1 . .
H25A C25 H25B 107.3 . .
C28 C26 C27 118.2(3) . .
C28 C26 C25 122.0(2) . .
C27 C26 C25 119.8(2) . .
C29 C27 C26 120.9(3) . .
C29 C27 H27 119.6 . .
C26 C27 H27 119.6 . .
C30 C28 C26 121.0(3) . .
C30 C28 H28 119.5 . .
C26 C28 H28 119.5 . .
C27 C29 C31 120.8(3) . .
C27 C29 H29 119.6 . .
C31 C29 H29 119.6 . .
C28 C30 C31 120.7(3) . .
C28 C30 H30 119.7 . .
C31 C30 H30 119.7 . .
C30 C31 C29 118.4(3) . .
C30 C31 C32 121.9(3) . .
C29 C31 C32 119.7(2) . .
C31 C32 P2 116.29(19) . .
C31 C32 H32A 108.2 . .
P2 C32 H32A 108.2 . .
C31 C32 H32B 108.2 . .
P2 C32 H32B 108.2 . .
H32A C32 H32B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.708(2) .
Mo1 O3 1.714(2) .
Mo1 O4 1.909(2) .
Mo1 O1 1.964(2) .
Mo1 O5 2.226(2) .
Mo1 O23 2.321(2) 2_746
Mo2 O7 1.714(2) .
Mo2 O6 1.715(2) .
Mo2 O8 1.900(2) .
Mo2 O4 1.911(2) .
Mo2 O9 2.341(2) .
Mo2 O23 2.341(2) 2_746
Mo3 O11 1.701(2) .
Mo3 O10 1.713(2) .
Mo3 O8 1.917(2) .
Mo3 O12 1.955(2) .
Mo3 O22 2.2088(19) 2_746
Mo3 O9 2.439(2) .
Mo4 O14 1.697(2) .
Mo4 O13 1.757(2) .
Mo4 O12 1.881(2) .
Mo4 O16 1.937(2) .
Mo4 O15 2.192(2) .
Mo4 O22 2.3542(19) 2_746
Mo5 O17 1.691(2) .
Mo5 O18 1.759(2) .
Mo5 O1 1.904(2) .
Mo5 O16 1.931(2) .
Mo5 O21 2.200(2) 2_746
Mo5 O5 2.366(2) .
Cu1 O18 1.941(2) .
Cu1 O19 1.954(2) .
Cu1 N2 1.981(3) .
Cu1 N1 2.007(3) .
Cu1 O20 2.268(3) .
Cu2 O13 1.918(2) .
Cu2 N3 1.981(2) .
Cu2 N4 1.996(2) .
Cu2 O24 2.002(2) .
Cu2 O25 2.262(3) .
P1 O15 1.518(2) .
P1 O5 1.548(2) .
P1 O9 1.548(2) .
P1 C25 1.802(3) .
P2 O21 1.513(2) .
P2 O22 1.543(2) .
P2 O23 1.546(2) .
P2 C32 1.799(3) .
O19 H19C 0.807(19) .
O19 H19D 0.837(19) .
O20 H20C 0.844(19) .
O20 H20D 0.844(19) .
O21 Mo5 2.200(2) 2_756
O22 Mo3 2.2088(19) 2_756
O22 Mo4 2.3542(19) 2_756
O23 Mo1 2.321(2) 2_756
O23 Mo2 2.341(2) 2_756
O24 H24C 0.829(19) .
O24 H24D 0.820(19) .
O25 H25C 0.829(19) .
O25 H25D 0.818(19) .
O90 H90A 0.852(19) .
O90 H90B 0.854(19) .
O91 H91A 0.855(19) .
O91 H91B 0.861(19) .
O92 H92A 0.77(5) .
O92 H92B 0.80(5) .
O93 H93A 0.837(19) .
O93 H93B 0.837(19) .
N1 C1 1.326(4) .
N1 C4 1.356(4) .
N2 C10 1.333(4) .
N2 C9 1.363(4) .
N3 C13 1.326(4) .
N3 C17 1.357(4) .
N4 C24 1.325(4) .
N4 C18 1.360(4) .
C1 C2 1.411(4) .
C1 H1 0.9300 .
C2 C3 1.366(5) .
C2 H2 0.9300 .
C3 C5 1.410(5) .
C3 H3 0.9300 .
C4 C5 1.409(4) .
C4 C9 1.426(4) .
C5 C6 1.436(4) .
C6 C7 1.364(5) .
C6 H6 0.9300 .
C7 C8 1.436(4) .
C7 H7 0.9300 .
C8 C9 1.401(4) .
C8 C12 1.410(5) .
C10 C11 1.403(4) .
C10 H10 0.9300 .
C11 C12 1.380(5) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.397(4) .
C13 H13 0.9300 .
C14 C15 1.370(5) .
C14 H14 0.9300 .
C15 C16 1.412(4) .
C15 H15 0.9300 .
C16 C17 1.406(4) .
C16 C19 1.433(4) .
C17 C18 1.433(4) .
C18 C21 1.395(4) .
C19 C20 1.357(5) .
C19 H19A 0.9300 .
C20 C21 1.440(4) .
C20 H20A 0.9300 .
C21 C22 1.409(4) .
C22 C23 1.377(5) .
C22 H22 0.9300 .
C23 C24 1.405(4) .
C23 H23 0.9300 .
C24 H24 0.9300 .
C25 C26 1.519(4) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 C28 1.397(4) .
C26 C27 1.398(4) .
C27 C29 1.392(4) .
C27 H27 0.9300 .
C28 C30 1.394(4) .
C28 H28 0.9300 .
C29 C31 1.397(4) .
C29 H29 0.9300 .
C30 C31 1.396(4) .
C30 H30 0.9300 .
C31 C32 1.515(4) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
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
O15 P1 O5 Mo1 172.62(14) . .
O9 P1 O5 Mo1 49.34(18) . .
C25 P1 O5 Mo1 -67.60(17) . .
O15 P1 O5 Mo5 9.1(2) . .
O9 P1 O5 Mo5 -114.15(16) . .
C25 P1 O5 Mo5 128.91(16) . .
O7 Mo2 O8 Mo3 -76.63(14) . .
O6 Mo2 O8 Mo3 177.04(13) . .
O4 Mo2 O8 Mo3 51.0(2) . .
O9 Mo2 O8 Mo3 5.16(11) . .
O23 Mo2 O8 Mo3 89.27(12) 2_746 .
O15 P1 O9 Mo2 -153.05(12) . .
O5 P1 O9 Mo2 -31.30(17) . .
C25 P1 O9 Mo2 86.23(16) . .
O15 P1 O9 Mo3 -29.42(17) . .
O5 P1 O9 Mo3 92.33(15) . .
C25 P1 O9 Mo3 -150.14(14) . .
O14 Mo4 O12 Mo3 174.35(12) . .
O13 Mo4 O12 Mo3 -82.38(13) . .
O16 Mo4 O12 Mo3 36.2(2) . .
O15 Mo4 O12 Mo3 89.75(12) . .
O22 Mo4 O12 Mo3 -3.00(10) 2_746 .
O14 Mo4 O13 Cu2 -11.8(3) . .
O12 Mo4 O13 Cu2 -116.7(3) . .
O16 Mo4 O13 Cu2 91.6(3) . .
O22 Mo4 O13 Cu2 173.8(3) 2_746 .
O5 P1 O15 Mo4 -63.24(15) . .
O9 P1 O15 Mo4 59.89(15) . .
C25 P1 O15 Mo4 178.55(12) . .
O17 Mo5 O18 Cu1 -8.5(3) . .
O1 Mo5 O18 Cu1 -113.5(3) . .
O16 Mo5 O18 Cu1 95.6(3) . .
O5 Mo5 O18 Cu1 177.1(3) . .
O22 P2 O21 Mo5 -63.25(15) . 2_756
O23 P2 O21 Mo5 59.98(16) . 2_756
C32 P2 O21 Mo5 177.55(12) . 2_756
O21 P2 O22 Mo3 176.00(13) . 2_756
O23 P2 O22 Mo3 52.41(18) . 2_756
C32 P2 O22 Mo3 -64.16(18) . 2_756
O21 P2 O22 Mo4 10.7(2) . 2_756
O23 P2 O22 Mo4 -112.87(16) . 2_756
C32 P2 O22 Mo4 130.56(16) . 2_756
O21 P2 O23 Mo1 -26.57(18) . 2_756
O22 P2 O23 Mo1 95.12(15) . 2_756
C32 P2 O23 Mo1 -146.51(14) . 2_756
O21 P2 O23 Mo2 -153.73(12) . 2_756
O22 P2 O23 Mo2 -32.04(17) . 2_756
C32 P2 O23 Mo2 86.33(16) . 2_756
C4 N1 C1 C2 -0.4(4) . .
Cu1 N1 C1 C2 176.6(2) . .
N1 C1 C2 C3 -1.6(5) . .
C1 C2 C3 C5 1.0(5) . .
C1 N1 C4 C5 2.9(4) . .
Cu1 N1 C4 C5 -174.6(2) . .
C1 N1 C4 C9 -178.9(3) . .
Cu1 N1 C4 C9 3.6(3) . .
N1 C4 C5 C3 -3.4(4) . .
C9 C4 C5 C3 178.5(3) . .
N1 C4 C5 C6 176.8(3) . .
C9 C4 C5 C6 -1.3(4) . .
C2 C3 C5 C4 1.3(4) . .
C2 C3 C5 C6 -178.9(3) . .
C4 C5 C6 C7 1.2(4) . .
C3 C5 C6 C7 -178.6(3) . .
C5 C6 C7 C8 -0.9(5) . .
C6 C7 C8 C9 0.7(4) . .
C6 C7 C8 C12 -176.8(3) . .
C10 N2 C9 C8 2.0(4) . .
Cu1 N2 C9 C8 172.8(2) . .
C10 N2 C9 C4 -176.2(3) . .
Cu1 N2 C9 C4 -5.3(3) . .
C12 C8 C9 N2 -1.2(4) . .
C7 C8 C9 N2 -178.9(3) . .
C12 C8 C9 C4 176.8(3) . .
C7 C8 C9 C4 -0.8(4) . .
N1 C4 C9 N2 1.1(4) . .
C5 C4 C9 N2 179.4(3) . .
N1 C4 C9 C8 -177.1(3) . .
C5 C4 C9 C8 1.2(4) . .
C9 N2 C10 C11 -0.8(4) . .
Cu1 N2 C10 C11 -170.0(2) . .
N2 C10 C11 C12 -1.1(5) . .
C10 C11 C12 C8 1.8(5) . .
C9 C8 C12 C11 -0.7(4) . .
C7 C8 C12 C11 176.8(3) . .
C17 N3 C13 C14 -0.7(4) . .
Cu2 N3 C13 C14 178.2(2) . .
N3 C13 C14 C15 -2.2(5) . .
C13 C14 C15 C16 2.3(5) . .
C14 C15 C16 C17 0.4(4) . .
C14 C15 C16 C19 178.4(3) . .
C13 N3 C17 C16 3.7(4) . .
Cu2 N3 C17 C16 -175.5(2) . .
C13 N3 C17 C18 -174.2(3) . .
Cu2 N3 C17 C18 6.6(3) . .
C15 C16 C17 N3 -3.5(4) . .
C19 C16 C17 N3 178.3(3) . .
C15 C16 C17 C18 174.4(3) . .
C19 C16 C17 C18 -3.8(4) . .
C24 N4 C18 C21 -3.1(4) . .
Cu2 N4 C18 C21 173.1(2) . .
C24 N4 C18 C17 176.4(3) . .
Cu2 N4 C18 C17 -7.4(3) . .
N3 C17 C18 N4 0.6(4) . .
C16 C17 C18 N4 -177.4(3) . .
N3 C17 C18 C21 -179.9(3) . .
C16 C17 C18 C21 2.1(4) . .
C17 C16 C19 C20 2.2(4) . .
C15 C16 C19 C20 -175.8(3) . .
C16 C19 C20 C21 1.3(5) . .
N4 C18 C21 C22 3.0(4) . .
C17 C18 C21 C22 -176.5(3) . .
N4 C18 C21 C20 -179.2(3) . .
C17 C18 C21 C20 1.3(4) . .
C19 C20 C21 C18 -3.0(4) . .
C19 C20 C21 C22 174.7(3) . .
C18 C21 C22 C23 -0.1(4) . .
C20 C21 C22 C23 -177.8(3) . .
C21 C22 C23 C24 -2.5(4) . .
C18 N4 C24 C23 0.3(4) . .
Cu2 N4 C24 C23 -175.1(2) . .
C22 C23 C24 N4 2.5(5) . .
O15 P1 C25 C26 53.9(2) . .
O5 P1 C25 C26 -64.9(2) . .
O9 P1 C25 C26 175.3(2) . .
P1 C25 C26 C28 71.2(3) . .
P1 C25 C26 C27 -110.4(3) . .
C28 C26 C27 C29 -0.4(4) . .
C25 C26 C27 C29 -178.8(3) . .
C27 C26 C28 C30 -0.7(4) . .
C25 C26 C28 C30 177.8(3) . .
C26 C27 C29 C31 1.0(4) . .
C26 C28 C30 C31 1.0(4) . .
C28 C30 C31 C29 -0.4(4) . .
C28 C30 C31 C32 177.5(3) . .
C27 C29 C31 C30 -0.6(4) . .
C27 C29 C31 C32 -178.6(3) . .
C30 C31 C32 P2 76.0(3) . .
C29 C31 C32 P2 -106.2(3) . .
O21 P2 C32 C31 47.3(2) . .
O22 P2 C32 C31 -71.6(2) . .
O23 P2 C32 C31 168.5(2) . .
