Directed Synthesis of Chromium and Molybdenum Metallaborane Clusters. Preparation and Characterization of (Cp*Cr)2B5H9, (Cp*Mo)2B5H9, and (Cp*MoCl)2B4H10
Simon Aldridge; Thomas P. Fehlner; Maoyu Shang; Journal of the American Chemical Society 119 (1997) 2339–2340; doi:10.1021/ja963864m

data_4116936
_publ_section_title
;
 Directed Synthesis of Chromium and Molybdenum Metallaborane Clusters.
 Preparation and Characterization of (Cp*Cr)2B5H9, (Cp*Mo)2B5H9, and
 (Cp*MoCl)2B4H10
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2339
_journal_page_last               2340
_journal_paper_doi               10.1021/ja963864m
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C20 H40 B4 Cl2 Mo2'
_chemical_formula_weight         586.54
_chemical_name_systematic
; 
 (Me5CpMo)2Cl2(B4H10) 
;
_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'
_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                 103.183(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5162(11)
_cell_length_b                   15.261(2)
_cell_length_c                   14.815(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      6
_cell_volume                     2535.1(5)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL_V5 (Siemens, 1994)'
_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       \q/2\q
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3717
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.00003(27)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.216
_refine_ls_goodness_of_fit_obs   1.289
_refine_ls_hydrogen_treatment
;
 Methyl hydrogen atoms were idealized with riding model, borane ones imposed
 bond length constraints.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.240
_refine_ls_restrained_S_obs      1.286
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_obs          0.0708
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+20.2601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2290
_refine_ls_wR_factor_obs         0.2148
_reflns_number_observed          2910
_reflns_number_total             3523
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja963864m.cif
_cod_data_source_block           JA963864M-302
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+20.2601P] 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^)+(0.1122P)^2^+20.2601P] 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               4116936