Unprecedented Cage-Carbon to Cage-Boron NMe3 Transfer in a Monocarbon Molybdenacarborane
Shaowu Du; Jason A. Kautz; Thomas D. McGrath; F. Gordon A. Stone; Inorganic Chemistry 41 (2002) 3202–3211; doi:10.1021/ic020091w

data_4318106
_publ_contact_author_address
; Department of Chemistry
   Baylor University
   PO Box 97348
   Waco
   TX, 76798-7348
;
_publ_contact_author_email       Gordon_Stone@baylor.edu
_publ_contact_author_fax         '254 710 2403'
_publ_contact_author_name        'Prof. F. Gordon A. Stone'
_publ_contact_author_phone       '254 710 4427'
_publ_section_title
;
 Unprecedented Cage-Carbon to Cage-Boron NMe3 Transfer in a Monocarbon
 Molybdenacarborane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3202
_journal_page_last               3211
_journal_paper_doi               10.1021/ic020091w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C21 H46 B10 Br2 Mo N4'
_chemical_formula_weight         718.48
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                93.883(9)
_cell_angle_beta                 103.008(9)
_cell_angle_gamma                114.451(7)
_cell_formula_units_Z            2
_cell_length_a                   11.0575(9)
_cell_length_b                   12.3036(11)
_cell_length_c                   14.726(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1747.5(4)
_computing_cell_refinement       'Enraf-Nonius CAD4 (1989)'
_computing_data_collection       'Enraf-Nonius CAD4 (1989)'
_computing_data_reduction        'XCAD4 Siemens Software (Harms, 1993)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Bruker, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6544
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.680
_exptl_absorpt_correction_T_max  0.6351
_exptl_absorpt_correction_T_min  0.4088
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            brick-red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         .500
_refine_diff_density_min         -.593
_refine_diff_density_rms         .070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.144
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.3979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4472
_reflns_number_total             6193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020091w_4.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.3979P] 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^)+(0.0322P)^2^+1.3979P] 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        1747.5(3)
_cod_database_code               4318106