Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]manganese(II)} dodecamolybdo(V,VI)phosphate hexahydrate
Hao, Lujiang; Ma, Chunling; Chen, Jianghui; Zhang, Xiaofei; Zhang, Xiutang; Acta Crystallographica Section E 66 (2010) m231–m232; doi:10.1107/S160053681000320X

data_2225138
_publ_section_title
;
 Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]manganese(II)}
 dodecamolybdo(V,VI)phosphate hexahydrate
;
_journal_coeditor_code           WM2301
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m231
_journal_page_last               m232
_journal_paper_doi               10.1107/S160053681000320X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mn (C8 H7 N3)3]2 [P Mo12 O40], 6H2 O'
_chemical_formula_moiety         '2(C24 H21 Mn N9 2+), Mo12 O40 P 4-, 6(H2 O)'
_chemical_formula_sum            'C48 H54 Mn2 Mo12 N18 O46 P'
_chemical_formula_weight         2911.22
_chemical_name_systematic
;
Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]manganese(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                 104.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.897(4)
_cell_length_b                   16.360(3)
_cell_length_c                   27.615(6)
_cell_measurement_reflns_used    7042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.92
_cell_volume                     8250(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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15879
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  0.8452
_exptl_absorpt_correction_T_min  0.7802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5620
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.517
_refine_diff_density_min         -0.589
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+43.0549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                5890
_reflns_number_total             7042
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2301.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               2225138
_cod_database_fobs_code          2225138