C-H Activation of Terminal Alkynes by Tris-(3,5-dimethylpyrazolyl)boraterhodiumneopentylisocyanide: New Metal-Carbon Bond Strengths
Gyeongshin Choi; James Morris; William W. Brennessel; William D. Jones; Journal of the American Chemical Society 134 (2012) 9276–9284; doi:10.1021/ja301095r

data_4118006
_publ_contact_author_address
;
 'Department of Chemistry, University of Rochester, Rochester,  New York 14627'
;
_publ_contact_author_email       jones@chem.rochester.edu
_publ_contact_author_name        'William D. Jones'
_publ_section_title
;
 C-H Activation of Terminal Alkynes by
 Tris-(3,5-dimethylpyrazolyl)boraterhodiumneopentylisocyanide: New
 Metal-Carbon Bond Strengths
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9276
_journal_page_last               9284
_journal_paper_doi               10.1021/ja301095r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C26 H42 B Cl N7 Rh Si, C6 H6'
_chemical_formula_sum            'C32 H48 B Cl N7 Rh Si'
_chemical_formula_weight         708.03
_chemical_name_common            jongc04
_chemical_name_systematic
; 
 Tp'Rh(CNneopentyl)(CCSiMe3)Cl
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.9666(13)
_cell_length_b                   11.1947(7)
_cell_length_c                   32.531(2)
_cell_measurement_reflns_used    4041
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      35.58
_cell_measurement_theta_min      2.73
_cell_volume                     7271.3(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            260153
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_correction_T_min  0.8294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         19509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0528P)^2^+2.1984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                11665
_reflns_number_total             19509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301095r_si_002_2.cif
_cod_data_source_block           3a-Cl
_cod_database_code               4118006