Tris{aquabis[3-(2-pyridyl)-1<i>H</i>-pyrazole]copper(II)} di-μ~9~-arsenato-hexatriaconta-μ~2~-oxido-octadecaoxidooctadecamolybdate(VI)
Zhang, Xiutang; Wei, Peihai; Shi, Congwen; Li, Bin; Hu, Bo; Acta Crystallographica Section E 66 (2010) m174–m175; doi:10.1107/S160053681000156X

data_2225130
_publ_section_title
;Tris{aquabis[3-(2-pyridyl)-1<i>H</i>-pyrazole]copper(II)}
 di-\m~9~-arsenato-hexatriaconta-\m~2~-oxido-octadecaoxidooctadecamolybdate(VI)
;
_journal_coeditor_code           WM2290
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m174
_journal_page_last               m175
_journal_paper_doi               10.1107/S160053681000156X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu (C8 H7 N3)2 (H2 O)]3 [As2 Mo18 O62]'
_chemical_formula_moiety         '3(C16 H16 Cu N6 O 2+), As2 Mo18 O62 6-'
_chemical_formula_sum            'C48 H48 As2 Cu3 Mo18 N18 O65'
_chemical_formula_weight         3984.45
_chemical_name_systematic
;Tris{aquabis[3-(2-pyridyl)-1<i>H</i>-pyrazole]copper(II)}
di-\m~9~-arsenato-hexatriaconta-\m~2~-oxido-octadecaoxidooctadecamolybdate(VI)
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.967(3)
_cell_length_b                   21.967(3)
_cell_length_c                   34.411(7)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.60
_cell_volume                     14380(4)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            25458
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.7554
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11346
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.248
_refine_diff_density_min         -1.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0630P)^2^+278.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                2053
_reflns_number_total             2750
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2290.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 'Hexagonal' changed to 'hexagonal'
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      'R -3c'
_cod_database_code               2225130
_cod_database_fobs_code          2225130