#------------------------------------------------------------------------------
#$Date: 2016-08-07 12:09:17 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/98/7039816.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_7039816
loop_
_publ_author_name
'Wang, Xiuli'
'Sun, Junjun'
'Lin, Hongyan'
'Chang, Zhihan'
'Wang, Xiang'
'Liu, Guocheng'
_publ_section_title
;
 A series of Anderson-type polyoxometalate-based metal-organic complexes:
 their pH-dependent electrochemical behaviour, and as electrocatalysts and
 photocatalysts.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12465
_journal_page_last               12478
_journal_paper_doi               10.1039/c6dt02216b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C30 H46 Cu Mo8 N8 O36'
_chemical_formula_weight         1925.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                96.1480(10)
_cell_angle_beta                 108.4720(10)
_cell_angle_gamma                96.0900(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8220(5)
_cell_length_b                   12.0750(7)
_cell_length_c                   13.6300(8)
_cell_measurement_reflns_used    6326
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2415
_cell_measurement_theta_min      2.4481
_cell_volume                     1354.04(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9877
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.246
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8  March, 1995'
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             935
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0271
_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)+(0.0310P)²+2.1781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5626
_reflns_number_total             6688
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02216b2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 7039813--7039819.cif.'
_cod_database_code               7039816
_shelx_shelxl_version_number     2014/7
_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   0.599
_shelx_estimated_absorpt_t_max   0.726
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
Mo1 Mo 0.70102(3) 0.69127(2) 0.64354(2) 0.03273(8) Uani 1 1 d . . .
Cu1 Cu 1.0000 0.5000 1.0000 0.03047(12) Uani 1 2 d S . P
N1 N 0.9247(3) 0.3364(2) 0.9884(2) 0.0320(6) Uani 1 1 d . . .
O1 O 0.7953(3) 0.49771(19) 0.83489(17) 0.0349(5) Uani 1 1 d . . .
C1 C 0.9225(4) 0.2911(3) 1.0736(2) 0.0384(8) Uani 1 1 d . . .
H1A H 0.9557 0.3375 1.1378 0.046 Uiso 1 1 calc R U .
O1W O 1.1656(3) 0.4614(2) 0.9356(2) 0.0453(6) Uani 1 1 d . . .
H1WA H 1.2547 0.4632 0.9540 0.038(11) Uiso 1 1 d R . .
H1WB H 1.1527 0.4474 0.8681 0.11(2) Uiso 1 1 d R . .
Mo2 Mo 0.43290(3) 0.69599(2) 0.40163(2) 0.02561(7) Uani 1 1 d . . .
O2 O 0.5264(3) 0.5214(2) 0.88499(18) 0.0434(6) Uani 1 1 d . . .
N2 N 0.7907(4) -0.0681(2) 1.0396(2) 0.0409(7) Uani 1 1 d . . .
H2B H 0.8537 -0.0309 1.0983 0.049 Uiso 1 1 calc R U .
C2 C 0.8724(4) 0.1773(3) 1.0693(3) 0.0395(8) Uani 1 1 d . . .
H2A H 0.8749 0.1478 1.1300 0.047 Uiso 1 1 calc R U .
O2W O 0.3846(4) 0.7997(3) 0.7700(2) 0.0645(8) Uani 1 1 d . . .
H2WA H 0.4817 0.8405 0.8009 0.055(13) Uiso 1 1 d R . .
H2WB H 0.4401 0.7374 0.7743 0.072(15) Uiso 1 1 d R . .
Mo3 Mo 0.32603(3) 0.51671(2) 0.53402(2) 0.02419(6) Uani 1 1 d . . .
O3 O 0.6224(3) 0.66161(18) 0.75522(16) 0.0326(5) Uani 1 1 d . . .
N3 N 1.2250(4) -0.1493(3) 1.5836(3) 0.0443(7) Uani 1 1 d . . .
H3A H 1.2943 -0.1580 1.6419 0.053 Uiso 1 1 calc R U .
C3 C 0.8188(4) 0.1083(3) 0.9736(2) 0.0322(6) Uani 1 1 d . . .
O3W O 1.1034(4) 0.4195(3) 0.7353(2) 0.0725(10) Uani 1 1 d . . .
H61 H 1.0273 0.3909 0.6793 0.087 Uiso 1 1 d R U .
H62 H 1.1786 0.4534 0.7182 0.087 Uiso 1 1 d R U .
Mo4 Mo 0.59499(3) 0.50982(2) 0.78150(2) 0.02569(7) Uani 1 1 d . . .
N4 N 0.7438(4) -0.1640(3) 1.2618(3) 0.0524(9) Uani 1 1 d . . .
H4B H 0.7323 -0.2246 1.2883 0.063 Uiso 1 1 calc R U .
O4 O 0.8971(3) 0.6717(3) 0.69214(19) 0.0523(7) Uani 1 1 d . . .
C4 C 0.8215(4) 0.1559(3) 0.8861(3) 0.0349(7) Uani 1 1 d . . .
H4A H 0.7875 0.1116 0.8207 0.042 Uiso 1 1 calc R U .
O5 O 0.7055(4) 0.8323(2) 0.6484(2) 0.0595(9) Uani 1 1 d . . .
C5 C 0.8747(4) 0.2690(3) 0.8964(2) 0.0337(7) Uani 1 1 d . . .
H5A H 0.8760 0.2999 0.8369 0.040 Uiso 1 1 calc R U .
O6 O 0.5991(2) 0.49866(16) 0.60146(15) 0.0234(4) Uani 1 1 d . . .
C6 C 0.7504(5) -0.0142(3) 0.9571(3) 0.0412(8) Uani 1 1 d . . .
O7 O 0.3448(3) 0.5258(2) 0.66771(17) 0.0343(5) Uani 1 1 d . . .
C7 C 0.7341(5) -0.1869(3) 1.0359(3) 0.0467(9) Uani 1 1 d . . .
H7A H 0.8208 -0.2203 1.0806 0.056 Uiso 1 1 calc R U .
H7B H 0.7073 -0.2252 0.9650 0.056 Uiso 1 1 calc R U .
O8 O 0.6792(2) 0.64572(18) 0.49263(16) 0.0290(4) Uani 1 1 d . . .
C8 C 0.5876(5) -0.2054(4) 1.0706(4) 0.0547(11) Uani 1 1 d . . .
H8A H 0.4961 -0.1837 1.0190 0.082 Uiso 1 1 calc R U .
H8B H 0.5624 -0.2852 1.0726 0.082 Uiso 1 1 calc R U .
C9 C 0.6088(5) -0.1408(4) 1.1764(4) 0.0579(11) Uani 1 1 d . . .
H9A H 0.6234 -0.0609 1.1722 0.087 Uiso 1 1 calc R U .
H9B H 0.5102 -0.1582 1.1926 0.087 Uiso 1 1 calc R U .
O10 O 0.4873(3) 0.64336(18) 0.28191(16) 0.0295(4) Uani 1 1 d . . .
C10 C 0.8841(4) -0.0958(3) 1.3008(3) 0.0406(8) Uani 1 1 d . . .
O11 O 0.5194(3) 0.83273(19) 0.42528(19) 0.0455(6) Uani 1 1 d . . .
C11 C 1.0041(4) -0.1201(3) 1.4003(3) 0.0359(7) Uani 1 1 d . . .
O12 O 0.2312(3) 0.6983(2) 0.34778(18) 0.0368(5) Uani 1 1 d . . .
C12 C 0.9664(4) -0.1989(3) 1.4594(3) 0.0461(9) Uani 1 1 d . . .
H12A H 0.8648 -0.2424 1.4368 0.055 Uiso 1 1 calc R U .
O13 O 0.4299(3) 0.67028(17) 0.54349(15) 0.0276(4) Uani 1 1 d . . .
C13 C 1.0798(5) -0.2120(3) 1.5510(3) 0.0471(9) Uani 1 1 d . . .
H13A H 1.0555 -0.2648 1.5907 0.056 Uiso 1 1 calc R U .
O14 O 0.1328(3) 0.5302(2) 0.4715(2) 0.0437(6) Uani 1 1 d . . .
C14 C 1.2666(5) -0.0733(3) 1.5287(3) 0.0462(9) Uani 1 1 d . . .
H14A H 1.3697 -0.0317 1.5530 0.055 Uiso 1 1 calc R U .
O15 O 0.9171(4) -0.0129(2) 1.2627(2) 0.0617(8) Uani 1 1 d . . .
C15 C 1.1569(4) -0.0567(3) 1.4366(3) 0.0413(8) Uani 1 1 d . . .
H15A H 1.1848 -0.0032 1.3985 0.050 Uiso 1 1 calc R U .
O16 O 0.6597(5) -0.0580(3) 0.8707(3) 0.0852(13) Uani 1 1 d . . .
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
O5 Mo1 O4 105.47(16) . .
O5 Mo1 O3 102.28(13) . .
O4 Mo1 O3 102.14(11) . .
O5 Mo1 O8 100.73(11) . .
O4 Mo1 O8 95.29(11) . .
O3 Mo1 O8 146.08(9) . .
O5 Mo1 O13 88.03(12) . .
O4 Mo1 O13 162.90(12) . .
O3 Mo1 O13 84.74(8) . .
O8 Mo1 O13 71.48(8) . .
O5 Mo1 O6 159.46(12) . .
O4 Mo1 O6 94.73(11) . .
O3 Mo1 O6 76.54(8) . .
O8 Mo1 O6 73.18(7) . .
O13 Mo1 O6 71.43(7) . .
N1 Cu1 N1 180.0 2_767 .
N1 Cu1 O1W 89.17(11) 2_767 2_767
N1 Cu1 O1W 90.83(11) . 2_767
N1 Cu1 O1W 90.83(11) 2_767 .
N1 Cu1 O1W 89.17(11) . .
O1W Cu1 O1W 180.00(12) 2_767 .
N1 Cu1 O1 92.28(9) 2_767 .
N1 Cu1 O1 87.72(9) . .
O1W Cu1 O1 86.27(9) 2_767 .
O1W Cu1 O1 93.73(9) . .
N1 Cu1 O1 87.72(9) 2_767 2_767
N1 Cu1 O1 92.28(9) . 2_767
O1W Cu1 O1 93.73(9) 2_767 2_767
O1W Cu1 O1 86.27(9) . 2_767
O1 Cu1 O1 180.0 . 2_767
C5 N1 C1 118.3(3) . .
C5 N1 Cu1 121.4(2) . .
C1 N1 Cu1 120.3(2) . .
Mo4 O1 Cu1 141.40(13) . .
N1 C1 C2 122.3(3) . .
O11 Mo2 O12 105.07(13) . .
O11 Mo2 O10 100.44(11) . .
O12 Mo2 O10 101.54(10) . .
O11 Mo2 O13 101.50(10) . .
O12 Mo2 O13 96.52(10) . .
O10 Mo2 O13 146.74(9) . .
O11 Mo2 O8 89.95(11) . .
O12 Mo2 O8 162.77(9) . .
O10 Mo2 O8 83.56(8) . .
O13 Mo2 O8 71.79(8) . .
O11 Mo2 O6 161.19(11) . 2_666
O12 Mo2 O6 93.62(9) . 2_666
O10 Mo2 O6 77.34(8) . 2_666
O13 Mo2 O6 73.83(8) . 2_666
O8 Mo2 O6 71.26(7) . 2_666
O11 Mo2 Mo3 136.59(9) . .
O12 Mo2 Mo3 84.65(8) . .
O10 Mo2 Mo3 119.25(6) . .
O13 Mo2 Mo3 35.13(6) . .
O8 Mo2 Mo3 78.55(5) . .
O6 Mo2 Mo3 41.92(5) 2_666 .
C6 N2 C7 123.6(3) . .
C3 C2 C1 119.1(3) . .
O14 Mo3 O7 105.51(11) . .
O14 Mo3 O8 101.77(12) . 2_666
O7 Mo3 O8 96.95(10) . 2_666
O14 Mo3 O13 99.92(11) . .
O7 Mo3 O13 95.87(10) . .
O8 Mo3 O13 150.78(9) 2_666 .
O14 Mo3 O6 96.86(10) . 2_666
O7 Mo3 O6 157.62(9) . 2_666
O8 Mo3 O6 79.04(8) 2_666 2_666
O13 Mo3 O6 79.13(8) . 2_666
O14 Mo3 O6 173.08(10) . .
O7 Mo3 O6 81.37(9) . .
O8 Mo3 O6 77.83(8) 2_666 .
O13 Mo3 O6 78.29(8) . .
O6 Mo3 O6 76.26(8) 2_666 .
O14 Mo3 Mo2 88.20(8) . .
O7 Mo3 Mo2 131.98(8) . .
O8 Mo3 Mo2 125.55(6) 2_666 .
O13 Mo3 Mo2 36.10(6) . .
O6 Mo3 Mo2 46.53(5) 2_666 .
O6 Mo3 Mo2 86.51(4) . .
Mo4 O3 Mo1 118.33(12) . .
C13 N3 C14 122.2(3) . .
C2 C3 C4 118.1(3) . .
C2 C3 C6 124.4(3) . .
C4 C3 C6 117.5(3) . .
O2 Mo4 O1 104.66(12) . .
O2 Mo4 O3 102.97(11) . .
O1 Mo4 O3 97.81(10) . .
O2 Mo4 O10 102.34(11) . 2_666
O1 Mo4 O10 99.18(10) . 2_666
O3 Mo4 O10 144.67(9) . 2_666
O2 Mo4 O7 91.43(10) . .
O1 Mo4 O7 163.88(9) . .
O3 Mo4 O7 77.14(9) . .
O10 Mo4 O7 77.98(9) 2_666 .
O2 Mo4 O6 160.72(10) . .
O1 Mo4 O6 94.62(9) . .
O3 Mo4 O6 73.82(8) . .
O10 Mo4 O6 74.11(7) 2_666 .
O7 Mo4 O6 69.29(7) . .
C10 N4 C9 123.0(3) . .
C5 C4 C3 119.6(3) . .
N1 C5 C4 122.6(3) . .
Mo3 O6 Mo2 91.55(7) 2_666 2_666
Mo3 O6 Mo3 103.74(8) 2_666 .
Mo2 O6 Mo3 97.74(7) 2_666 .
Mo3 O6 Mo1 91.87(7) 2_666 .
Mo2 O6 Mo1 163.27(9) 2_666 .
Mo3 O6 Mo1 97.34(7) . .
Mo3 O6 Mo4 163.40(9) 2_666 .
Mo2 O6 Mo4 85.77(6) 2_666 .
Mo3 O6 Mo4 92.86(7) . .
Mo1 O6 Mo4 86.29(7) . .
O16 C6 N2 123.7(3) . .
O16 C6 C3 119.1(3) . .
N2 C6 C3 117.2(3) . .
Mo3 O7 Mo4 116.47(11) . .
N2 C7 C8 112.9(3) . .
Mo3 O8 Mo1 109.14(9) 2_666 .
Mo3 O8 Mo2 110.70(9) 2_666 .
Mo1 O8 Mo2 103.54(10) . .
C9 C8 C7 114.1(3) . .
N4 C9 C8 114.8(4) . .
Mo2 O10 Mo4 116.97(10) . 2_666
O15 C10 N4 123.3(4) . .
O15 C10 C11 119.2(3) . .
N4 C10 C11 117.3(3) . .
C15 C11 C12 118.6(3) . .
C15 C11 C10 118.1(3) . .
C12 C11 C10 123.2(3) . .
C13 C12 C11 119.5(3) . .
Mo3 O13 Mo2 108.77(10) . .
Mo3 O13 Mo1 110.37(9) . .
Mo2 O13 Mo1 103.91(9) . .
N3 C13 C12 120.2(3) . .
N3 C14 C15 119.8(3) . .
C14 C15 C11 119.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O5 1.693(3) .
Mo1 O4 1.698(3) .
Mo1 O3 1.913(2) .
Mo1 O8 2.014(2) .
Mo1 O13 2.318(2) .
Mo1 O6 2.3432(19) .
Cu1 N1 1.990(3) 2_767
Cu1 N1 1.990(3) .
Cu1 O1W 1.997(3) 2_767
Cu1 O1W 1.997(3) .
Cu1 O1 2.393(2) .
Cu1 O1 2.393(2) 2_767
N1 C5 1.336(4) .
N1 C1 1.341(4) .
O1 Mo4 1.713(2) .
C1 C2 1.387(5) .
Mo2 O11 1.696(2) .
Mo2 O12 1.701(2) .
Mo2 O10 1.907(2) .
Mo2 O13 1.999(2) .
Mo2 O8 2.315(2) .
Mo2 O6 2.3317(19) 2_666
Mo2 Mo3 3.2115(3) .
O2 Mo4 1.700(2) .
N2 C6 1.329(4) .
N2 C7 1.459(4) .
C2 C3 1.383(5) .
Mo3 O14 1.681(2) .
Mo3 O7 1.767(2) .
Mo3 O8 1.949(2) 2_666
Mo3 O13 1.952(2) .
Mo3 O6 2.1463(19) 2_666
Mo3 O6 2.3337(19) .
O3 Mo4 1.910(2) .
N3 C13 1.331(5) .
N3 C14 1.337(5) .
C3 C4 1.385(4) .
C3 C6 1.501(5) .
Mo4 O10 1.916(2) 2_666
Mo4 O7 2.302(2) .
Mo4 O6 2.4552(19) .
N4 C10 1.329(5) .
N4 C9 1.454(5) .
C4 C5 1.373(5) .
O6 Mo3 2.1464(19) 2_666
O6 Mo2 2.3316(19) 2_666
C6 O16 1.219(4) .
C7 C8 1.514(6) .
O8 Mo3 1.949(2) 2_666
C8 C9 1.509(7) .
O10 Mo4 1.916(2) 2_666
C10 O15 1.226(4) .
C10 C11 1.512(5) .
C11 C15 1.388(5) .
C11 C12 1.390(5) .
C12 C13 1.368(5) .
C14 C15 1.371(5) .
