A 4-ethylpyridine complex of tetrachloromolybdenum(III) and its oxidation product
Modec, Barbara; Brenčič, Jurij V.; Golič, Ljubo; Acta Crystallographica Section C 56 (2000) 780–782; doi:10.1107/S0108270100004911

data_2011149
_publ_section_title
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 A 4-ethylpyridine complex of tetrachloromolybdenum(III) and its
 oxidation product
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              780
_journal_page_last               782
_journal_paper_doi               10.1107/S0108270100004911
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '(C6 H16 N1) [Mo Cl4 (C7 H9 N)2]'
_chemical_formula_moiety         'C6 H16 N1 1+, C14 H18 Cl4 Mo N2 1-'
_chemical_formula_sum            'C20 H34 Cl4 Mo N3'
_chemical_formula_weight         554.24
_chemical_name_systematic
;
triethylammonium cis-tetrachlorodi(4-ethylpyridine)molybdenum(III)
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7025(9)
_cell_length_b                   7.766(2)
_cell_length_c                   16.7929(6)
_cell_measurement_reflns_used    12687
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      3.75
_cell_volume                     2569.5(7)
_computing_cell_refinement       d*trek
_computing_data_collection
'd*trek (Molecular Structure Corporation, 1997)'
_computing_data_reduction        d*trek
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.14
_diffrn_measurement_device_type  'Quantum CCD Rigaku AFC7'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_av_sigmaI/netI    .0419
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18043
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    .937
_exptl_absorpt_correction_T_max  .869
_exptl_absorpt_correction_T_min  .739
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(REQABA; Jacobson, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .15
_refine_diff_density_max         .813
_refine_diff_density_min         -.486
_refine_ls_abs_structure_details 'Flack, 1983'
_refine_ls_abs_structure_Flack   -.03(4)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4069
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_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          .047
_refine_ls_R_factor_gt           .029
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0285P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .059
_reflns_number_gt                3267
_reflns_number_total             5860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            na1469.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0285P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0285P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2569.6(6)
_cod_database_code               2011149
_cod_database_fobs_code          2011149