#------------------------------------------------------------------------------
#$Date: 2017-07-14 06:38:43 +0300 (Fri, 14 Jul 2017) $
#$Revision: 198712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/65/1546537.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_1546537
loop_
_publ_author_name
'Chen, Yongdong'
'Zhang, Chaolei'
'Caoping, Yang'
'Zhang, Jiangwei'
'zheng, Kai'
'Fang, Qihua'
'Li, Gao'
_publ_section_title
;
 Waugh type [CoMo9O32]6- cluster with atomically dispersed Co3+ derives
 from Anderson type [CoMo6O24]3- for photocatalytic oxygen molecule
 activation
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR04373B
_journal_year                    2017
_chemical_formula_moiety         'Co H8 Mo6 O24, 8(H2 O), (H4 N)'
_chemical_formula_sum            'Co H28 Mo6 N O32'
_chemical_formula_weight         1188.78
_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_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.432(2)
_cell_length_b                   10.997(2)
_cell_length_c                   11.725(2)
_cell_measurement_reflns_used    3293
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      3.302
_cell_volume                     1452.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         3.302
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.0094(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3293
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0757P)²+7.8400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3060
_reflns_number_total             3293
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nr04373b2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        1452.2(5)
_cod_database_code               1546537
_shelxl_version_number           2013-4
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6
 0.9 with sigma of 0.02
 H2A-H2B \\sim H2A-H2C \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O15(H15A,H15B), N2(H2A,H2B), O13(H13A,H13B), O14(H14A,H14B)
3.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), O0AA(H0AA)
;
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 0.0000 0.0156(3) Uani 1 2 d S T P . .
Mo3 Mo -0.15844(5) -0.23377(5) 0.06938(5) 0.0227(2) Uani 1 1 d . . . . .
Mo1 Mo -0.13557(5) 0.24532(4) -0.12043(4) 0.0221(2) Uani 1 1 d . . . . .
Mo2 Mo -0.29498(5) 0.01514(5) -0.04726(5) 0.0243(2) Uani 1 1 d . . . . .
O2 O -0.1205(4) 0.1099(4) 0.0306(3) 0.0182(8) Uani 1 1 d . . . . .
H2 H -0.1136 0.1430 0.1091 0.022 Uiso 1 1 calc R . . . .
O5 O -0.2540(4) -0.0926(4) 0.0842(4) 0.0264(9) Uani 1 1 d . . . . .
O3 O 0.1307(4) 0.0986(4) 0.0730(3) 0.0192(8) Uani 1 1 d . . . . .
H3 H 0.1280 0.1308 0.1504 0.023 Uiso 1 1 calc R . . . .
O11 O -0.2547(5) -0.3194(5) -0.0254(4) 0.0385(12) Uani 1 1 d . . . . .
O12 O -0.1567(5) -0.2949(5) 0.2046(4) 0.0364(12) Uani 1 1 d . . . . .
O6 O 0.0132(4) 0.3059(4) -0.0345(4) 0.0241(9) Uani 1 1 d D . . . .
H6 H 0.025(7) 0.376(4) 0.006(6) 0.029 Uiso 1 1 d DR . . . .
O7 O -0.1295(5) 0.3020(5) -0.2553(4) 0.0360(11) Uani 1 1 d . . . . .
O9 O -0.3928(5) -0.0713(5) -0.1400(5) 0.0415(13) Uani 1 1 d . . . . .
O1 O 0.0055(4) 0.1031(4) -0.1310(3) 0.0193(8) Uani 1 1 d . . . . .
H0AA H 0.0043 0.0633 -0.2059 0.03(2) Uiso 1 1 calc R . . . .
O4 O -0.2443(4) 0.1145(4) -0.1659(4) 0.0270(10) Uani 1 1 d . . . . .
O8 O -0.2245(5) 0.3443(5) -0.0605(5) 0.0364(11) Uani 1 1 d . . . . .
O10 O -0.3793(5) 0.1164(5) 0.0146(5) 0.0399(12) Uani 1 1 d . . . . .
O16 O -0.0158(10) 0.0415(6) -0.3481(5) 0.081(3) Uani 1 1 d . . . A 2
H1A H 0.0527 0.0733 -0.3416 0.121 Uiso 1 1 d G . . A 2
H1B H -0.0198 -0.0198 -0.3928 0.121 Uiso 1 1 d G . . A 2
O15 O -0.3320(8) -0.5395(8) 0.1100(6) 0.068(2) Uani 1 1 d . . . . .
H15A H -0.3216 -0.5779 0.1739 0.102 Uiso 1 1 d G . . . .
H15B H -0.3247 -0.4636 0.1231 0.102 Uiso 1 1 d G . . . .
N1 N -0.3568(9) -0.0125(9) 0.2685(8) 0.063(2) Uani 1 1 d . . . . .
H2A H -0.3021 -0.0353 0.2325 0.095 Uiso 1 1 d DG . . . .
H2B H -0.3921 -0.0744 0.2896 0.095 Uiso 1 1 d DG . . . .
O13 O -0.5085(10) -0.2068(11) 0.2963(14) 0.117(4) Uani 1 1 d . . . . .
H13A H -0.5089 -0.2770 0.3267 0.176 Uiso 1 1 d G . . . .
H13B H -0.4395 -0.1914 0.2822 0.176 Uiso 1 1 d G . . . .
O14 O -0.4938(10) -0.3397(12) 0.0881(14) 0.140(5) Uani 1 1 d . . . B 2
H14A H -0.4857 -0.4165 0.0862 0.209 Uiso 1 1 d G . . B 2
H14B H -0.4631 -0.3075 0.0342 0.209 Uiso 1 1 d G . . B 2
H2C H -0.400(11) 0.039(9) 0.236(14) 2(3) Uiso 1 1 d D . . . .
H2D H -0.317(12) 0.019(12) 0.336(10) 0.14(7) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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'
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'
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 Co1 O2 180.0 3 .
O2 Co1 O3 95.14(18) . .
O2 Co1 O3 84.86(18) 3 .
O2 Co1 O3 84.86(18) . 3
O2 Co1 O3 95.14(18) 3 3
O2 Co1 O1 95.74(17) 3 .
O2 Co1 O1 84.26(17) 3 3
O2 Co1 O1 95.74(17) . 3
O2 Co1 O1 84.26(17) . .
O3 Co1 O3 180.0 . 3
O1 Co1 O3 83.89(17) . .
O1 Co1 O3 83.89(17) 3 3
O1 Co1 O3 96.11(17) 3 .
O1 Co1 O3 96.11(17) . 3
O1 Co1 O1 180.0 . 3
O5 Mo3 O3 72.24(16) . 3
O5 Mo3 O6 150.06(18) . 3
O5 Mo3 O1 83.09(18) . 3
O11 Mo3 O5 101.0(2) . .
O11 Mo3 O3 92.2(2) . 3
O11 Mo3 O12 106.8(3) . .
O11 Mo3 O6 96.7(2) . 3
O11 Mo3 O1 157.9(2) . 3
O12 Mo3 O5 98.6(2) . .
O12 Mo3 O3 160.4(2) . 3
O12 Mo3 O6 99.1(2) . 3
O12 Mo3 O1 93.8(2) . 3
O6 Mo3 O3 83.22(16) 3 3
O6 Mo3 O1 71.82(16) 3 3
O1 Mo3 O3 68.23(14) 3 3
O6 Mo1 O2 83.03(16) . .
O6 Mo1 O1 72.34(16) . .
O7 Mo1 O2 159.8(2) . .
O7 Mo1 O6 100.6(2) . .
O7 Mo1 O1 93.4(2) . .
O7 Mo1 O4 98.2(2) . .
O7 Mo1 O8 105.5(3) . .
O1 Mo1 O2 68.56(14) . .
O4 Mo1 O2 71.80(16) . .
O4 Mo1 O6 150.62(18) . .
O4 Mo1 O1 84.27(18) . .
O8 Mo1 O2 93.8(2) . .
O8 Mo1 O6 95.6(2) . .
O8 Mo1 O1 159.3(2) . .
O8 Mo1 O4 100.9(2) . .
O2 Mo2 O3 68.23(14) . 3
O5 Mo2 O2 83.46(17) . .
O5 Mo2 O3 71.51(17) . 3
O9 Mo2 O2 159.2(2) . .
O9 Mo2 O5 102.0(2) . .
O9 Mo2 O3 94.2(2) . 3
O9 Mo2 O4 95.8(2) . .
O9 Mo2 O10 106.1(3) . .
O4 Mo2 O2 71.51(16) . .
O4 Mo2 O5 148.94(19) . .
O4 Mo2 O3 82.08(17) . 3
O10 Mo2 O2 92.9(2) . .
O10 Mo2 O5 97.9(2) . .
O10 Mo2 O3 158.9(2) . 3
O10 Mo2 O4 101.4(2) . .
Co1 O2 Mo1 103.08(17) . .
Co1 O2 Mo2 104.06(17) . .
Co1 O2 H2 117.8 . .
Mo1 O2 H2 117.8 . .
Mo2 O2 Mo1 92.41(14) . .
Mo2 O2 H2 117.8 . .
Mo3 O5 Mo2 119.0(2) . .
Co1 O3 Mo3 103.58(16) . 3
Co1 O3 Mo2 102.86(17) . 3
Co1 O3 H3 118.0 . .
Mo3 O3 Mo2 92.24(15) 3 3
Mo3 O3 H3 118.0 3 .
Mo2 O3 H3 118.0 3 .
Mo3 O6 H6 114(5) 3 .
Mo1 O6 Mo3 117.0(2) . 3
Mo1 O6 H6 127(5) . .
Co1 O1 Mo3 104.30(18) . 3
Co1 O1 Mo1 104.08(17) . .
Co1 O1 H0AA 117.2 . .
Mo3 O1 H0AA 117.2 3 .
Mo1 O1 Mo3 93.55(15) . 3
Mo1 O1 H0AA 117.2 . .
Mo1 O4 Mo2 118.9(2) . .
H1A O16 H1B 109.5 . .
H15A O15 H15B 109.5 . .
H2A N1 H2B 109.5 . .
H2A N1 H2C 114.7 . .
H2A N1 H2D 104.2 . .
H2B N1 H2C 114.7 . .
H2B N1 H2D 104.1 . .
H2C N1 H2D 108(3) . .
H13A O13 H13B 109.4 . .
H14A O14 H14B 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 1.912(4) 3
Co1 O2 1.912(4) .
Co1 O3 1.925(4) 3
Co1 O3 1.925(4) .
Co1 O1 1.918(4) 3
Co1 O1 1.918(4) .
Mo3 O5 1.923(5) .
Mo3 O3 2.297(4) 3
Mo3 O11 1.706(5) .
Mo3 O12 1.718(5) .
Mo3 O6 1.946(5) 3
Mo3 O1 2.283(4) 3
Mo1 O2 2.297(4) .
Mo1 O6 1.940(5) .
Mo1 O7 1.712(5) .
Mo1 O1 2.265(4) .
Mo1 O4 1.916(5) .
Mo1 O8 1.719(5) .
Mo2 O2 2.297(4) .
Mo2 O5 1.937(4) .
Mo2 O3 2.319(4) 3
Mo2 O9 1.709(5) .
Mo2 O4 1.934(4) .
Mo2 O10 1.712(5) .
O2 H2 0.9800 .
O3 Mo3 2.297(4) 3
O3 Mo2 2.319(4) 3
O3 H3 0.9800 .
O6 Mo3 1.946(5) 3
O6 H6 0.90(2) .
O1 Mo3 2.283(4) 3
O1 H0AA 0.9800 .
O16 H1A 0.8499 .
O16 H1B 0.8502 .
O15 H15A 0.8502 .
O15 H15B 0.8500 .
N1 H2A 0.8496 .
N1 H2B 0.8493 .
N1 H2C 0.80(7) .
N1 H2D 0.91(9) .
O13 H13A 0.8502 .
O13 H13B 0.8503 .
O14 H14A 0.8503 .
O14 H14B 0.8503 .
