Bridging Rhodium‒Iron Borataaminocarbyne Complexes Formed by Intramolecular Isonitrile‒Borane Coordination
Cowie, Bradley E.; Emslie, David J. H.; Organometallics 32 (2013) 7297–; doi:10.1021/om4007483

data_4082078
_publ_section_title
;
 Bridging Rhodium--Iron Borataaminocarbyne Complexes Formed by
 Intramolecular Isonitrile--Borane Coordination
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7297
_journal_paper_doi               10.1021/om4007483
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C63 H62 B Fe N O2 P Rh S, 5(C7 H8)'
_chemical_formula_sum            'C98 H102 B Fe N O2 P Rh S'
_chemical_formula_weight         1654.4
_chemical_name_systematic
;
 brad19
;
_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
_cell_angle_alpha                92.065(2)
_cell_angle_beta                 98.126(2)
_cell_angle_gamma                104.399(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5439(13)
_cell_length_b                   14.7174(16)
_cell_length_c                   23.728(3)
_cell_measurement_reflns_used    8671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     3854.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.1353
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35237
_diffrn_reflns_theta_full        26.6
_diffrn_reflns_theta_max         26.6
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.7469
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
One molecule of disordered solvent (toluene) was removed from the lattice using Platon SQUEEZE.
;
_refine_diff_density_max         2.086
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         15693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+6.7627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.194
_reflns_number_gt                10428
_reflns_number_total             15693
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4007483_si_002.cif
_cod_data_source_block           brad19
_cod_original_cell_volume        3854.8(7)
_cod_database_code               4082078