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_4082077
_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_formula_moiety         'C61 H57 B Cl Fe N O2 P Rh S, 2(C6 H14)'
_chemical_formula_sum            'C73 H85 B Cl Fe N O2 P Rh S'
_chemical_formula_weight         1266.36
_chemical_name_systematic
;
 brad08
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 99.332(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.776(2)
_cell_length_b                   17.235(2)
_cell_length_c                   21.196(3)
_cell_measurement_reflns_used    2364
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.32
_cell_volume                     6407.9(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83485
_diffrn_reflns_theta_full        28.65
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.9616
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
One molecule of disordered solvent (hexane) was removed from the lattice using Platon SQUEEZE.
;
_refine_diff_density_max         1.425
_refine_diff_density_min         -1.1
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         16335
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+3.7949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                12493
_reflns_number_total             16335
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4007483_si_002.cif
_cod_data_source_block           brad08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6407.7(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4082077