#------------------------------------------------------------------------------
#$Date: 2016-08-07 12:09:17 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/98/7039814.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_7039814
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            'C7 H17 Cu Mo4 N2 O19'
_chemical_formula_weight         880.53
_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                99.444(4)
_cell_angle_beta                 97.040(3)
_cell_angle_gamma                109.631(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7790(13)
_cell_length_b                   10.2490(18)
_cell_length_c                   14.418(2)
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.3007
_cell_measurement_theta_min      2.3280
_cell_volume                     1048.3(3)
_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 0.998
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7796
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         2.162
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8  March, 1995'
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    2.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.472
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0495
_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)+(0.0649P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3879
_reflns_number_total             5243
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02216b2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
'Adding full bibliography for 7039813--7039819.cif.'
_cod_database_code               7039814
_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   0.448
_shelx_estimated_absorpt_t_max   0.578
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
Mo1 Mo 0.19278(8) 1.11914(6) 0.47585(4) 0.01353(14) Uani 1 1 d . .
Cu1 Cu 0.28953(14) 0.46579(11) 0.26724(7) 0.0268(2) Uani 1 1 d . .
O1 O 0.1225(6) 1.0394(5) 0.5842(3) 0.0154(10) Uani 1 1 d . .
N1 N 0.2378(9) 0.4569(7) 0.1254(5) 0.0283(15) Uani 1 1 d . .
O1W O 0.5551(8) 0.5830(6) 0.2766(4) 0.0350(14) Uani 1 1 d . .
H1WA H 0.4915 0.5154 0.2293 0.042 Uiso 1 1 d R U
H1WB H 0.5820 0.5466 0.3226 0.042 Uiso 1 1 d R U
C1 C 0.3090(11) 0.5709(8) 0.0892(6) 0.0273(17) Uani 1 1 d . .
H1A H 0.3783 0.6573 0.1312 0.033 Uiso 1 1 calc R U
Mo2 Mo 0.10727(8) 1.04684(7) 0.74297(4) 0.01555(15) Uani 1 1 d . .
O2 O 0.0412(7) 0.9982(6) 0.8439(3) 0.0247(12) Uani 1 1 d . .
O2W O 0.3691(10) 0.2793(7) 0.2504(5) 0.0483(19) Uani 1 1 d . .
H2WA H 0.3587 0.2138 0.2870 0.058 Uiso 1 1 d R U
H2WB H 0.4411 0.2570 0.2327 0.058 Uiso 1 1 d R U
C2 C 0.2842(11) 0.5662(8) -0.0076(5) 0.0241(16) Uani 1 1 d . .
N2 N 0.4494(19) 0.8150(9) 0.0113(7) 0.094(5) Uani 1 1 d . .
H2A H 0.4504 0.8159 0.0711 0.112 Uiso 1 1 calc R U
Mo3 Mo 0.24141(8) 0.86662(7) 0.57437(4) 0.01486(15) Uani 1 1 d . .
O3 O -0.0004(6) 1.1893(5) 0.7289(3) 0.0180(10) Uani 1 1 d . .
O3W O 0.3332(9) 0.4904(7) 0.4115(4) 0.0434(16) Uani 1 1 d . .
H3WA H 0.3126 0.5586 0.4414 0.052 Uiso 1 1 d R U
H3WB H 0.2373 0.4237 0.3986 0.052 Uiso 1 1 d R U
C3 C 0.1804(13) 0.4373(10) -0.0693(6) 0.039(2) Uani 1 1 d . .
H3A H 0.1635 0.4298 -0.1352 0.047 Uiso 1 1 calc R U
Mo4 Mo 0.26499(8) 0.88044(7) 0.30478(4) 0.01650(15) Uani 1 1 d . .
O4 O 0.0684(7) 1.2360(5) 0.4801(4) 0.0207(11) Uani 1 1 d . .
O4W O 0.0206(8) 0.3726(7) 0.2614(4) 0.0379(15) Uani 1 1 d . .
H4WA H -0.0106 0.2848 0.2617 0.045 Uiso 1 1 d R U
H4WB H -0.0264 0.4448 0.2617 0.045 Uiso 1 1 d R U
C4 C 0.3680(13) 0.6951(10) -0.0477(6) 0.035(2) Uani 1 1 d . .
O5 O 0.1817(6) 1.0716(5) 0.3414(3) 0.0166(10) Uani 1 1 d . .
C5 C 0.1355(12) 0.3329(9) 0.0672(6) 0.0324(19) Uani 1 1 d . .
H5A H 0.0852 0.2537 0.0925 0.039 Uiso 1 1 calc R U
O5W O 0.8610(11) 0.5443(9) 0.3525(6) 0.071(3) Uani 1 1 d . .
H50 H 0.8532 0.4938 0.3942 0.085 Uiso 1 1 d R U
H51 H 0.9105 0.6309 0.3819 0.085 Uiso 1 1 d R U
O6 O 0.4756(6) 0.9777(6) 0.6255(3) 0.0218(11) Uani 1 1 d . .
C6 C 0.541(3) 0.9512(13) -0.0143(11) 0.099(6) Uani 1 1 d . .
H6B H 0.6716 0.9895 0.0162 0.119 Uiso 1 1 calc R U
H6A H 0.5344 0.9358 -0.0831 0.119 Uiso 1 1 calc R U
O7 O 0.4149(7) 1.2284(6) 0.5183(4) 0.0236(11) Uani 1 1 d . .
C7 C 0.1025(14) 0.3204(10) -0.0324(6) 0.039(2) Uani 1 1 d . .
H7A H 0.0286 0.2338 -0.0730 0.047 Uiso 1 1 calc R U
O8 O 0.3186(8) 0.9177(6) 0.1987(4) 0.0276(12) Uani 1 1 d . .
O9 O 0.1492(6) 0.8719(5) 0.6910(3) 0.0163(10) Uani 1 1 d . .
O10 O 0.2407(7) 0.6992(6) 0.5496(4) 0.0269(12) Uani 1 1 d . .
O11 O 0.2332(6) 0.9184(5) 0.4550(3) 0.0158(10) Uani 1 1 d . .
O12 O 0.2903(8) 0.7230(6) 0.3077(4) 0.0272(12) Uani 1 1 d . .
O13 O 0.3652(13) 0.6810(9) -0.1333(5) 0.074(3) Uani 1 1 d . .
O14 O 0.3327(7) 1.1632(6) 0.7784(4) 0.0253(12) 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
O7 Mo1 O4 103.5(3) . .
O7 Mo1 O5 103.4(2) . .
O4 Mo1 O5 100.0(2) . .
O7 Mo1 O1 102.8(2) . .
O4 Mo1 O1 98.6(2) . .
O5 Mo1 O1 143.2(2) . .
O7 Mo1 O11 99.0(2) . .
O4 Mo1 O11 157.4(2) . .
O5 Mo1 O11 76.77(19) . .
O1 Mo1 O11 73.97(19) . .
O7 Mo1 O1 179.2(2) . 2_576
O4 Mo1 O1 77.3(2) . 2_576
O5 Mo1 O1 76.62(18) . 2_576
O1 Mo1 O1 76.83(19) . 2_576
O11 Mo1 O1 80.24(17) . 2_576
O4W Cu1 O1W 172.6(2) . .
O4W Cu1 N1 89.2(3) . .
O1W Cu1 N1 90.9(3) . .
O4W Cu1 O3W 89.7(3) . .
O1W Cu1 O3W 89.6(3) . .
N1 Cu1 O3W 174.6(3) . .
O4W Cu1 O2W 99.6(2) . .
O1W Cu1 O2W 87.8(2) . .
N1 Cu1 O2W 94.2(3) . .
O3W Cu1 O2W 91.2(3) . .
Mo1 O1 Mo3 101.89(19) . .
Mo1 O1 Mo2 155.0(3) . .
Mo3 O1 Mo2 92.87(17) . .
Mo1 O1 Mo1 103.17(19) . 2_576
Mo3 O1 Mo1 94.86(18) . 2_576
Mo2 O1 Mo1 95.45(16) . 2_576
C5 N1 C1 119.9(7) . .
C5 N1 Cu1 118.5(6) . .
C1 N1 Cu1 121.6(6) . .
N1 C1 C2 122.8(8) . .
O2 Mo2 O14 105.5(3) . .
O2 Mo2 O3 102.5(2) . .
O14 Mo2 O3 95.9(2) . .
O2 Mo2 O9 96.1(2) . .
O14 Mo2 O9 100.0(2) . .
O3 Mo2 O9 151.3(2) . .
O2 Mo2 O5 91.2(2) . 2_576
O14 Mo2 O5 162.2(2) . 2_576
O3 Mo2 O5 74.11(19) . 2_576
O9 Mo2 O5 83.90(19) . 2_576
O2 Mo2 O1 160.8(2) . .
O14 Mo2 O1 91.7(2) . .
O3 Mo2 O1 83.70(18) . .
O9 Mo2 O1 72.14(18) . .
O5 Mo2 O1 72.85(17) 2_576 .
C1 C2 C3 118.0(7) . .
C1 C2 C4 122.4(7) . .
C3 C2 C4 119.6(7) . .
C4 N2 C6 125.7(10) . .
O10 Mo3 O6 105.8(2) . .
O10 Mo3 O11 104.3(2) . .
O6 Mo3 O11 97.4(2) . .
O10 Mo3 O9 101.7(2) . .
O6 Mo3 O9 96.7(2) . .
O11 Mo3 O9 145.5(2) . .
O10 Mo3 O1 157.2(2) . .
O6 Mo3 O1 97.0(2) . .
O11 Mo3 O1 72.84(18) . .
O9 Mo3 O1 74.37(18) . .
O10 Mo3 O4 85.2(2) . 2_576
O6 Mo3 O4 168.7(2) . 2_576
O11 Mo3 O4 81.75(19) . 2_576
O9 Mo3 O4 78.37(19) . 2_576
O1 Mo3 O4 72.00(18) . 2_576
Mo4 O3 Mo2 115.3(2) 2_576 .
C7 C3 C2 119.4(8) . .
O12 Mo4 O8 105.5(3) . .
O12 Mo4 O3 97.8(2) . 2_576
O8 Mo4 O3 99.5(2) . 2_576
O12 Mo4 O6 101.3(2) . 2_676
O8 Mo4 O6 89.6(2) . 2_676
O3 Mo4 O6 155.7(2) 2_576 2_676
O12 Mo4 O11 93.5(2) . .
O8 Mo4 O11 158.7(2) . .
O3 Mo4 O11 87.19(19) 2_576 .
O6 Mo4 O11 77.03(18) 2_676 .
O12 Mo4 O5 160.8(2) . .
O8 Mo4 O5 93.1(2) . .
O3 Mo4 O5 74.03(18) 2_576 .
O6 Mo4 O5 83.11(19) 2_676 .
O11 Mo4 O5 69.17(17) . .
Mo1 O4 Mo3 115.8(3) . 2_576
O13 C4 N2 122.4(9) . .
O13 C4 C2 119.5(9) . .
N2 C4 C2 117.9(8) . .
Mo1 O5 Mo2 113.6(2) . 2_576
Mo1 O5 Mo4 109.7(2) . .
Mo2 O5 Mo4 92.21(18) 2_576 .
N1 C5 C7 120.5(8) . .
Mo3 O6 Mo4 173.5(3) . 2_676
C6 C6 N2 111.4(14) 2_675 .
C3 C7 C5 119.4(8) . .
Mo3 O9 Mo2 116.2(2) . .
Mo3 O11 Mo1 106.9(2) . .
Mo3 O11 Mo4 149.7(3) . .
Mo1 O11 Mo4 103.19(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O7 1.682(5) .
Mo1 O4 1.772(5) .
Mo1 O5 1.904(5) .
Mo1 O1 1.933(5) .
Mo1 O11 2.163(5) .
Mo1 O1 2.397(5) 2_576
Cu1 O4W 1.970(6) .
Cu1 O1W 1.985(6) .
Cu1 N1 2.017(7) .
Cu1 O3W 2.026(6) .
Cu1 O2W 2.185(6) .
O1 Mo3 2.250(5) .
O1 Mo2 2.296(4) .
O1 Mo1 2.397(5) 2_576
N1 C5 1.326(10) .
N1 C1 1.334(10) .
C1 C2 1.376(11) .
Mo2 O2 1.697(5) .
Mo2 O14 1.712(5) .
Mo2 O3 1.937(5) .
Mo2 O9 1.973(5) .
Mo2 O5 2.240(5) 2_576
C2 C3 1.382(11) .
C2 C4 1.506(11) .
N2 C4 1.279(12) .
N2 C6 1.469(13) .
Mo3 O10 1.692(5) .
Mo3 O6 1.777(5) .
Mo3 O11 1.883(5) .
Mo3 O9 1.907(5) .
Mo3 O4 2.257(5) 2_576
O3 Mo4 1.907(5) 2_576
C3 C7 1.373(13) .
Mo4 O12 1.696(5) .
Mo4 O8 1.703(5) .
Mo4 O3 1.907(5) 2_576
Mo4 O6 2.061(5) 2_676
Mo4 O11 2.196(4) .
Mo4 O5 2.266(5) .
O4 Mo3 2.257(5) 2_576
C4 O13 1.216(11) .
O5 Mo2 2.240(5) 2_576
C5 C7 1.404(11) .
O6 Mo4 2.062(5) 2_676
C6 C6 1.40(3) 2_675
