Tetra-μ-oxido-tetrakis{dioxido[3-(2-pyridyl)-1<i>H</i>-pyrazole]molybdenum(VI)}
Li, Dacheng; Liu, Ying; Wei, Peihai; Hu, Bo; Zhang, Xiutang; Acta Crystallographica Section E 65 (2009) m1074–; doi:10.1107/S1600536809031717

data_2223252
_publ_section_title
Tetra-\m-oxido-tetrakis{dioxido[3-(2-pyridyl)-1<i>H</i>-pyrazole]molybdenum(VI)}
_journal_coeditor_code           ZQ2001
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1074
_journal_paper_doi               10.1107/S1600536809031717
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mo4 O12 (C8 H7 N3)4]'
_chemical_formula_moiety         'C32 H28 Mo4 N12 O12'
_chemical_formula_sum            'C32 H28 Mo4 N12 O12'
_chemical_formula_weight         1156.42
_chemical_name_systematic
Tetra-\m-oxido-tetrakis{dioxido[3-(2-pyridyl)-1<i>H</i>-pyrazole]molybdenum(VI)}
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.4412(16)
_cell_length_b                   14.4412(16)
_cell_length_c                   9.094(2)
_cell_measurement_reflns_used    1675
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1896.5(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7579
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1675
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.00
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.024
_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^)+(0.0295P)^2^+2.0306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.056
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                1316
_reflns_number_total             1675
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zq2001.cif
_cod_data_source_block           I
_cod_original_cell_volume        1896.6(5)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               2223252
_cod_database_fobs_code          2223252