An Effective Strategy To Construct Novel Polyoxometalate-Based Hybrids by Deliberately Controlling Organic Ligand Transformation In Situ.
Wang, Xiu-Li; Zhang, Rui; Wang, Xiang; Lin, Hong-Yan; Liu, Guo-Cheng; Inorganic chemistry 55 (2016) 6384–6393; doi:10.1021/acs.inorgchem.6b00009

data_4347324
_publ_section_title
;
 An Effective Strategy To Construct Novel Polyoxometalate-Based Hybrids by
 Deliberately Controlling Organic Ligand Transformation In Situ.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6384
_journal_page_last               6393
_journal_paper_doi               10.1021/acs.inorgchem.6b00009
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C52 H36 Cu2 Mo12 N16 O48 P, 6(O)'
_chemical_formula_sum            'C52 H36 Cu2 Mo12 N16 O54 P'
_chemical_formula_weight         3058.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   18.001(5)
_cell_length_b                   18.001(5)
_cell_length_c                   12.946(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4195(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         1.600
_exptl_absorpt_coefficient_mu    2.358
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       block
_exptl_crystal_F_000             2938.0
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0381
_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/[\s^2^(Fo^2^)+(0.0572P)^2^+9.7756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3694
_reflns_number_total             5208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00009_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        4195(3)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4347324
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.637
_shelx_res_checksum              31073
_shelx_hkl_checksum              14975