Synthesis and Structure of a Carbene-Stabilized Boraallene Coordinated to Rhodium
Holger Braunschweig; Qing Ye; Krzysztof Radacki; Inorganic Chemistry 52 (2013) 5639–5641; doi:10.1021/ic4005505

data_4334956
_publ_contact_author_address
; Institut f\"ur Anorganische Chemie
Universit\"at W\"urzburg
Am Hubland
97074 W\"urzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-3184623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-3185260
_publ_section_title
;
 Synthesis and Structure of a Carbene-Stabilized Boraallene Coordinated to
 Rhodium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5639
_journal_page_last               5641
_journal_paper_doi               10.1021/ic4005505
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H66 B N3 P Rh Si2'
_chemical_formula_sum            'C36 H66 B N3 P Rh Si2'
_chemical_formula_weight         741.79
_chemical_name_common
;
?
;
_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-97
_cell_angle_alpha                75.854(7)
_cell_angle_beta                 86.561(7)
_cell_angle_gamma                76.536(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6199(17)
_cell_length_b                   13.047(2)
_cell_length_c                   15.053(2)
_cell_measurement_reflns_used    7959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.40
_cell_volume                     1966.9(5)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            151131
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.733
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7928
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+2.6862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                7177
_reflns_number_total             7928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4005505_si_002.cif
_cod_data_source_block           kr607
_cod_database_code               4334956