A second triclinic form of pyridinium μ-oxo-μ-sulfato-bis[oxotris(isothiocyanato)molybdate(V)]
Kamenar, Boris; Cindrić, Marina; Strukan, Neven; Acta Crystallographica Section C 50 (1994) 1396–1399; doi:10.1107/S0108270194004865

data_2010063
_publ_section_title
;
 A second triclinic form of pyridinium
 \m-oxo-\m-sulfato-bis[oxotris(isothiocyanato)molybdate(V)]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1396
_journal_page_last               1399
_journal_paper_doi               10.1107/S0108270194004865
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         '4C5 H6 N 1- , C6 Mo2 N6 O7 S7 4-'
_chemical_formula_structural     '(C5 H6 N)4 (Mo2 O3 (S O4) (N C S)6)'
_chemical_formula_sum            'C26 H24 Mo2 N10 O7 S7'
_chemical_formula_weight         1004.85
_chemical_name_systematic
;
\m-oxo-\m-sulfato-bis[oxotris(isothiocyanato)molybdate(V)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                93.45(2)
_cell_angle_beta                 95.13(4)
_cell_angle_gamma                96.44(2)
_cell_formula_units_Z            4
_cell_length_a                   8.2200(10)
_cell_length_b                   12.491(6)
_cell_length_c                   40.14(2)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      5
_cell_volume                     4069(3)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1992)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4S (Stoe & Cie, 1992)'
_computing_molecular_graphics    'PLUTON (Spek, 1982)'
_computing_publication_material  'SHELXL93; CSU (Vickovi\'c, 1988)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Philips PW1100 diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2963
_diffrn_reflns_av_sigmaI/netI    0.5566
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17372
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        10
_diffrn_standards_interval_time  70
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red-brown'
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.770
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.914
_refine_ls_goodness_of_fit_obs   1.227
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         14370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.3936
_refine_ls_R_factor_obs          0.0844
_refine_ls_shift/esd_max         -0.109
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.1633P)^2^]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.3889
_refine_ls_wR_factor_obs         0.348
_reflns_number_observed          3231
_reflns_number_total             14446
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1097.cif
_cod_data_source_block           1
_cod_database_code               2010063