Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural, Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich Metallacarboranes of Iron, Cobalt, and Nickel
Tomlinson, Susan; Zheng, Chong; Hosmane, Narayan S.; Yang, Jimin; Wang, Ying; Zhang, Hongming; Gray, Thomas G.; Demissie, Temesgen; Maguire, John A.; Baumann, Frank; Klein, Axel; Sarkar, Biprajit; Kaim, Wolfgang; Lipscomb, William N.; Organometallics 24 (2005) 2177–2187; doi:10.1021/om048982u

data_1100793
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights 
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural, 
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich 
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2177
_journal_page_last               2187
_journal_paper_doi               10.1021/om048982u
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C22 H60 B8 Fe2 N2 Si4'
_chemical_formula_weight         663.26
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.06(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.574(1)
_cell_length_b                   16.472(1)
_cell_length_c                   18.363(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      10.0
_cell_measurement_theta_min      5.0
_cell_volume                     3800.9(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'omega scans'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.041
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4887
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        3.26
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Siemens XEMP'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00142(17)
_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_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+5.7999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.090
_reflns_number_gt                3807
_reflns_number_total             4635
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4060287
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1100793