Synthesis of the first Metallasila-closo-dodecaborates(1-). Silaborate Complexes of Cobalt, Rhodium, and Iridium
Lars Wesemann; Yves Ramjoie; Michael Trinkaus; Beate Ganter; Inorganic Chemistry 36 (1997) 5192–5197; doi:10.1021/ic970455y

data_4323668
_publ_contact_author
;
     Dr. Lars Wesemann
     Institut fuer Anorganische Chemie
     RWTH Aachen
     Prof.-Pirlet-Str.1
     52074 Aachen
     Germany
;
_publ_contact_author_email       beate.ganter@ac.rwth-aachen.de
_publ_contact_author_fax         '(0241) 8888288'
_publ_contact_author_phone       '(0241) 804795'
_publ_section_title
;
 Synthesis of the first Metallasila-closo-dodecaborates(1-). Silaborate
 Complexes of Cobalt, Rhodium, and Iridium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5192
_journal_page_last               5197
_journal_paper_doi               10.1021/ic970455y
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'recrystall. from Et2O/THF'
_chemical_formula_sum            'C37 H60 B10 O P Rh Si'
_chemical_formula_weight         790.97
_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_type_scat_source           International_Tables_for_Xray_Crystallography
_audit_creation_date             20-03-97
_audit_creation_method           from_MolEN_master_file_using_cif_in
_cell_angle_alpha                92.68(2)
_cell_angle_beta                 90.22(3)
_cell_angle_gamma                96.77(3)
_cell_formula_units_Z            2.00
_cell_length_a                   9.838(4)
_cell_length_b                   11.312(3)
_cell_length_c                   18.858(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     2081.7(12)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Patterson
_diffrn_ambient_temperature      203
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \w
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7983
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -1.27
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.8470
_refine_diff_density_min         0.0000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.355
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.162
_refine_ls_R_factor_obs          0.063
_refine_ls_shift/esd_max         0.015
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.062
_reflns_number_observed          4612
_reflns_number_total             7701
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            ic970455y.cif
_cod_data_source_block           YR3_230297
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w = 4Fo^2^/
(\s^2^(Fo^2^) + 0.0016 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2082(2)
_cod_original_formula_sum        'C37 H60 B10 O1 P1 Rh1 Si1'
_cod_database_code               4323668