Assembly of three organic‒inorganic hybrid supramolecular materials based on reduced molybdenum(V) phosphates
Zhang, He; Yu, Kai; Lv, Jing-Hua; Wang, Chun-Mei; Wang, Chun-Xiao; Zhou, Bai-Bin; Journal of Solid State Chemistry 217 (2014) 22–30; doi:10.1016/j.jssc.2014.05.010

data_1562304
_publ_section_title
;
 Assembly of three organic--inorganic hybrid supramolecular materials
 based on reduced molybdenum(V) phosphates
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              22
_journal_page_last               30
_journal_paper_doi               10.1016/j.jssc.2014.05.010
_journal_volume                  217
_journal_year                    2014
_chemical_formula_sum            'C30 H61 Mo12 N12 Ni3 O73 P8'
_chemical_formula_weight         3333.02
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                90.057(3)
_cell_angle_beta                 96.118(3)
_cell_angle_gamma                94.984(3)
_cell_formula_units_Z            2
_cell_length_a                   13.676(3)
_cell_length_b                   14.029(3)
_cell_length_c                   23.714(5)
_cell_measurement_reflns_used    7584
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.89
_cell_volume                     4506.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22526
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_T_max  0.5026
_exptl_absorpt_correction_T_min  0.3115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3234
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.311
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1247
_refine_ls_number_reflns         15718
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+23.5147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                14062
_reflns_number_total             15868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-217-22.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_database_code               1562304