Dehydrogenation of Saturated CC and BN Bonds at Cationic N-Heterocyclic Carbene Stabilized M(III) Centers (M = Rh, Ir)
Christina Y. Tang; Amber L. Thompson; Simon Aldridge; Journal of the American Chemical Society 132 (2010) 10578–10591; doi:10.1021/ja1043787

data_4102756
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 Dehydrogenation of Saturated CC and BN Bonds at Cationic N-Heterocyclic
 Carbene Stabilized M(III) Centers (M = Rh, Ir)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10578
_journal_page_last               10591
_journal_paper_doi               10.1021/ja1043787
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C54 H72 Ir N4, C32 H12 B F24, 0.835(C5 H12)'
_chemical_formula_sum            'C90.18 H94.02 B F24 Ir N4'
_chemical_formula_weight         1892.84
_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
_audit_creation_date             09-10-30
_audit_creation_method           CRYSTALS_ver_12.90
_cell_angle_alpha                90
_cell_angle_beta                 92.21849(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4160(1)
_cell_length_b                   13.2405(1)
_cell_length_c                   39.2632(2)
_cell_measurement_reflns_used    20701
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     9047.17(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            109194
_diffrn_reflns_theta_full        26.651
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3844.212
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.86
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9125
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         20514
_refine_ls_number_restraints     236
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.0125358
_refine_ls_shift/su_mean         7.8303022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 11.4 15.9 7.45 1.92 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1002
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.1002
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              50
_reflns_limit_l_min              0
_reflns_number_gt                15204
_reflns_number_total             20514
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.81
_oxford_diffrn_Wilson_scale      115.69
_oxford_refine_ls_r_factor_ref   0.0600
_oxford_refine_ls_scale          0.100911(14)
_oxford_reflns_number_all        20514
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 005ct09
_cod_data_source_file            ja1043787_si_002_02.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C90.18 H94.02 B F24 Ir N4 '
_cod_database_code               4102756