Oxidation of Tricarbonylmolybdacarborane. 1. First Examples of Oxomolybda(VI)carboranes
Jae-Hak Kim; Eunkee Hong; Jinkwon Kim; Youngkyu Do; Inorganic Chemistry 35 (1996) 5112–5113; doi:10.1021/ic960223j

data_4323889
_publ_section_title
;
 Oxidation of Tricarbonylmolybdacarborane. 1. First Examples of
 Oxomolybda(VI)carboranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5112
_journal_page_last               5113
_journal_paper_doi               10.1021/ic960223j
_journal_volume                  35
_journal_year                    1996
_chemical_formula_analytical     'C24 H45 B9 Mo N2 O2 S2'
_chemical_formula_moiety         'C28 H53 B9 Mo N2 O3 S2'
_chemical_formula_structural     'C28 H53 B9 Mo N2 O3 S2'
_chemical_formula_sum            'C28 H53 B9 Mo N2 O3 S2'
_chemical_formula_weight         723.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2bc'
_symmetry_space_group_name_H-M   'P 1 1 21/b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                95.670(10)
_cell_formula_units_Z            4
_cell_length_a                   10.3070(10)
_cell_length_b                   19.069(4)
_cell_length_c                   19.608(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.33
_cell_measurement_theta_min      8.37
_cell_volume                     3835.0(10)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'MoleN (Enraf-Nonius, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4TSB'
_diffrn_measurement_method       omega/2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4639
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        37.5
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  '7200 sec '
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9814
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_obs          0.0714
_refine_ls_shift/esd_max         0.104
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.9593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1834
_refine_ls_wR_factor_obs         0.1571
_reflns_number_observed          3109
_reflns_number_total             4639
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960223j_1.cif
_cod_data_source_block           cbmosph2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.9593P] 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^)+(0.0906P)^2^+0.9593P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4323889