Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]cadmium(II)} dodecamolybdo(V,VI)phosphate hexahydrate
Hao, Lujiang; Wang, Yan; Zhang, Xiaofei; Chen, Jiangkui; Zhang, Xiutang; Acta Crystallographica Section E 66 (2010) m268–m269; doi:10.1107/S1600536810004307

data_2225398
_publ_section_title
;
 Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]cadmium(II)}
 dodecamolybdo(V,VI)phosphate hexahydrate
;
_journal_coeditor_code           WM2302
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m268
_journal_page_last               m269
_journal_paper_doi               10.1107/S1600536810004307
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cd (C8 H7 N3)3]2 [P Mo12 O40] , 6H2 O'
_chemical_formula_moiety         '2C24 H21 Cd N9 2+ , Mo12 O40 P 4- , 6H2O'
_chemical_formula_sum            'C48 H54 Cd2 Mo12 N18 O46 P'
_chemical_formula_weight         3026.14
_chemical_name_systematic
;
Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]cadmium(II)}
dodecamolybdo(V,VI)phosphate hexahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0326(14)
_cell_length_b                   16.4779(12)
_cell_length_c                   27.267(2)
_cell_measurement_reflns_used    5617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.46
_cell_volume                     8252.8(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21276
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.8321
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.816
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         7254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0570P)^2^+46.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                6211
_reflns_number_total             7254
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2302.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2225398
_cod_database_fobs_code          2225398