1,4-Dimethylpyridinium hexakis(dimethylformamide-κ<i>O</i>)calcium(II) dodecamolybdophosphate
Xue-Jie Tan; Si-Xiu Sun; Jian-Ping Ma; Lian-Dong Liu; Yu-Bin Dong; Wen-Tao Yu; Dian-Xiang Xing; Acta Crystallographica Section C 60 (2004) m476–m478; doi:10.1107/S0108270104019705

data_2014516
_publ_section_title
;
 1,4-Dimethylpyridinium
 hexakis(dimethylformamide-\k<i>O</i>)calcium(II)
 dodecamolybdophosphate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m476
_journal_page_last               m478
_journal_paper_doi               10.1107/S0108270104019705
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C7 H10 N) [Ca (C3 H7 N O)6] [P Mo12 O40]'
_chemical_formula_moiety
'C18 H42 Ca N6 O6 2+, C7 H10 N +, Mo12 O40 P 3-'
_chemical_formula_sum            'C25 H52 Ca Mo12 N7 O46 P'
_chemical_formula_weight         2409.07
_chemical_name_systematic
;
1,4-Dimethylpyridinium hexakis(dimethylformamide-\kO)calcium(II)
tetracontaoxophosphidododecamolybdate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.293(6)
_cell_length_b                   13.246(2)
_cell_length_c                   12.888(2)
_cell_measurement_reflns_used    380
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      7.5
_cell_volume                     6537.2(17)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39117
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        none
_diffrn_standards_number         'not applicable to area detectors'
_exptl_absorpt_coefficient_mu    2.426
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4632.0
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.628
_refine_ls_abs_structure_details 'Flack (1983), 6579 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         14090
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+11.3547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                12008
_reflns_number_total             14090
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1193.cif
_cod_data_source_block           I
_cod_original_cell_volume        6537.6(17)
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_original_formula_sum        'C25 H52 Ca Mo12 N7 O46 P '
_cod_database_code               2014516
_cod_database_fobs_code          2014516