Origins of Unsaturation in Group 6 Metallaboranes. Synthesis, Crystal Structure, and Molecular Orbital Calculations for (Cp*MoCl)2B3H7 (Cp* = Pentamethylcyclopentadienyl)
Simon Aldridge; Maoyu Shang; Thomas P. Fehlner; Journal of the American Chemical Society 119 (1997) 11120–11121; doi:10.1021/ja972685h

data_4117063
_publ_section_title
;
 Origins of Unsaturation in Group 6 Metallaboranes. Synthesis, Crystal
 Structure, and Molecular Orbital Calculations for (Cp*MoCl)2B3H7 (Cp* =
 Pentamethylcyclopentadienyl)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11120
_journal_page_last               11121
_journal_paper_doi               10.1021/ja972685h
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C20 H37 B3 Cl2 Mo2'
_chemical_formula_weight         572.71
_chemical_name_systematic
;
 (Me5CpMoCl)2B4H7
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   difmap
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5231(13)
_cell_length_b                   8.5231(13)
_cell_length_c                   32.956(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     2394.0(7)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'SDP_Package (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2422
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_correction_T_min  0.8225
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.143
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment
;
Cp ring hydrogen atoms refined with riding model, borane ones isotropically
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.0259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1053
_refine_ls_wR_factor_obs         0.0944
_reflns_number_observed          1826
_reflns_number_total             2099
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja972685h.cif
_cod_data_source_block           f9704
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.0259P] 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^)+(0.0506P)^2^+2.0259P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117063