An Unprecedented M-O Cluster Constructed from Nanosized {[C<sub>5</sub>NH<sub>5</sub>]<sub>9</sub>[H<sub>31</sub>Mo<sup>V</sup><sub>12</sub>O<sub>24</sub>Co<sup>II</sup><sub>12</sub>(PO<sub>4</sub>)<sub>23</sub>(H<sub>2</sub>O)<sub>4</sub>]}<sup>2-</sup> Anions Exhibiting Interesting Nonlinear-Optical Properties.
Dong, Yayu; Hu, Gonghao; Miao, Hao; He, Xingxiang; Fang, Min; Xu, Yan; Inorganic chemistry 55 (2016) 11621–11625; doi:10.1021/acs.inorgchem.6b02160

data_4349241
_publ_section_title
;
 An Unprecedented M-O Cluster Constructed from Nanosized
 {[C<sub>5</sub>NH<sub>5</sub>]<sub>9</sub>[H<sub>31</sub>Mo<sup>V</sup><sub>12</sub>O<sub>24</sub>Co<sup>II</sup><sub>12</sub>(PO<sub>4</sub>)<sub>23</sub>(H<sub>2</sub>O)<sub>4</sub>]}<sup>2-</sup>
 Anions Exhibiting Interesting Nonlinear-Optical Properties.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11621
_journal_page_last               11625
_journal_paper_doi               10.1021/acs.inorgchem.6b02160
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C91 H158 Co12 Mo12 N21 O132 P23'
_chemical_formula_weight         6229.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.692(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.916(13)
_cell_length_b                   21.039(7)
_cell_length_c                   28.447(10)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.23
_cell_volume                     20780(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74847
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.132
_exptl_absorpt_coefficient_mu    1.913
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             12320
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.726
_refine_diff_density_min         -2.056
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         19261
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+5.8283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14623
_reflns_number_total             19261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02160_si_002.cif
_cod_data_source_block           a01
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4349241
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              9404
_shelx_hkl_checksum              6197