Ammonium <i>cis</i>-tetrachlorobispyridinemolybdate(III)‒pyridine‒water (1/1/0.5)
Leban, Ivan; Modec, Barbara; Brenčič, Jurij V.; Acta Crystallographica Section C 50 (1994) 1546–1548; doi:10.1107/S0108270194005640

data_2010078
_publ_section_title
;
 Ammonium
 <i>cis</i>-tetrachlorobispyridinemolybdate(III)--pyridine--water
 (1/1/0.5)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1546
_journal_page_last               1548
_journal_paper_doi               10.1107/S0108270194005640
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical
;
(N H4 1+) (C10 H10 Cl4 N2 Mo 1-) (C5 H5 N) 0.5(H2 O)
;
_chemical_formula_sum            'C15 H20 Cl4 Mo N4 O0.5'
_chemical_formula_weight         502.1
_chemical_name_systematic
;
ammonium cis-tetrachlorobispyridinemolybdate(III)-pyridine-water(1:1:0.5)
;
_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'
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 97.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3840(10)
_cell_length_b                   32.637(4)
_cell_length_c                   8.8600(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     2118.2(5)
_computing_cell_refinement       'Enraf Nonius CAD-4'
_computing_data_collection       'Enraf Nonius CAD-4'
_computing_data_reduction
;
NRCVAX (Gabe, Le Page, Charland, Lee & White, 1989)
;
_computing_molecular_graphics
;
ORTEP (Johnson, 1971), PLUTON (Spek, 1991)
;
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w/2\q scan with variable rate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11881
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        2.27
_diffrn_standards_interval_time  '2 hours'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.940
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.307
_refine_ls_goodness_of_fit_obs   1.391
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.334
_refine_ls_restrained_S_obs      1.391
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_obs          0.058
_refine_ls_shift/esd_max         -0.274
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
 calc w = 1/[\s^2^(F~o~^2^)+(0.0001P)^2^+10.9983P]
where  P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1369
_refine_ls_wR_factor_obs         0.126
_reflns_number_observed          4307
_reflns_number_total             5599
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1190.cif
_cod_data_source_block           cisc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010078