Role of Coordination Geometry in Dictating the Barrier to Hydride Migration in d6 Square-Pyramidal Iridium and Rhodium Pincer Complexes
Michael Findlater; Alison Cartwright-Sykes; Peter S. White; Cynthia K. Schauer; Maurice Brookhart; Journal of the American Chemical Society 133 (2011) 12274–12284; doi:10.1021/ja204851x

data_4106516
_publ_contact_author_address
;
Department of Chemistry
University of North Carolina
Kenan Labs, CB3290
Chapel Hill, NC 27599
USA
;
_publ_contact_author_email       mbrookhart@unc.edu
_publ_contact_author_name        'Maurice Brookhart'
_publ_section_title
;
 Role of Coordination Geometry in Dictating the Barrier to Hydride
 Migration in d6 Square-Pyramidal Iridium and Rhodium Pincer Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12274
_journal_page_last               12284
_journal_paper_doi               10.1021/ja204851x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C25 H34 Ir O2 P2, C32 H12 B F24'
_chemical_formula_sum            'C57 H58 B F24 Ir O2 P2'
_chemical_formula_weight         1495.98
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_creation_method
;
manual editing of the .cif file
created by SHELXTL Ver. 6.10
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5388(4)
_cell_length_b                   12.5388(4)
_cell_length_c                   78.145(5)
_cell_measurement_temperature    100(2)
_cell_volume                     12286.1(10)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -89
_diffrn_reflns_number            102673
_diffrn_reflns_theta_full        62.57
_diffrn_reflns_theta_max         62.57
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    5.725
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             5952
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         9711
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+37.4416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                9695
_reflns_number_total             9711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204851x_si_002.cif
_cod_data_source_block           c06056
_cod_original_sg_symbol_Hall     P4abw2nw
_cod_database_code               4106516