Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]nickel(II)} dodecamolybdo(V,VI)phosphate hexahydrate
Hao, Lujiang; Liu, Tongjun; Chen, Jiangkui; Zhang, Xiaofei; Acta Crystallographica Section E 66 (2010) m319–m320; doi:10.1107/S1600536810005945

data_2225402
_publ_section_title
;
 Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]nickel(II)}
 dodecamolybdo(V,VI)phosphate hexahydrate
;
_journal_coeditor_code           WM2306
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m319
_journal_page_last               m320
_journal_paper_doi               10.1107/S1600536810005945
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C8 H7 N3)3]2 [P Mo12 O40], 6H2 O'
_chemical_formula_moiety         '2(C24 H21 N9 Ni), Mo12 O40 P, 6(H2 O)'
_chemical_formula_sum            'C48 H54 Mo12 N18 Ni2 O46 P'
_chemical_formula_weight         2918.76
_chemical_name_systematic
;
Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]nickel(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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.741(4)
_cell_length_b                   16.285(3)
_cell_length_c                   27.678(6)
_cell_measurement_reflns_used    7216
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.68
_cell_volume                     8202(3)
_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       '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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22802
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.6518
_exptl_absorpt_correction_T_min  0.4398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5644
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.667
_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         7216
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0880P)^2^+10.3967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                5310
_reflns_number_total             7216
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2306.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2225402
_cod_database_fobs_code          2225402