Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]iron(II)} tetradecamolybdo(V,VI)silicate
Wei, Peihai; Yuan, Dong; Zhu, Wencai; Zhang, Xiutang; Hu, Bo; Acta Crystallographica Section E 66 (2010) m190–m191; doi:10.1107/S1600536810002412

data_2225137
_publ_section_title
;
 Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]iron(II)}
 tetradecamolybdo(V,VI)silicate
;
_journal_coeditor_code           WM2300
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m190
_journal_page_last               m191
_journal_paper_doi               10.1107/S1600536810002412
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe (C8 H7 N3)3]2 [Si Mo14 O44]'
_chemical_formula_moiety         '2(C24 H21 Fe N9 2+), Mo14 O44 Si 4-'
_chemical_formula_sum            'C48 H42 Fe2 Mo14 N18 O44 Si'
_chemical_formula_weight         3057.95
_chemical_name_systematic
;
Bis{tris[3-(2-pyridyl)-1<i>H</i>-pyrazole]iron(II)}
tetradecamolybdo(V,VI)silicate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.055(3)
_cell_length_b                   16.931(3)
_cell_length_c                   18.562(4)
_cell_measurement_reflns_used    7026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.65
_cell_volume                     4002.6(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27223
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_T_max  0.8201
_exptl_absorpt_correction_T_min  0.7470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         7026
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0580P)^2^+47.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                4730
_reflns_number_total             7026
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2300.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_cell_volume        4002.6(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225137
_cod_database_fobs_code          2225137