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_4102765
_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         'C48 H66 B Ir N5, C32 H12 B F24 '
_chemical_formula_sum            'C80 H78 B2 F24 Ir N5'
_chemical_formula_weight         1779.33
_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
_audit_creation_date             09-10-28
_audit_creation_method           CRYSTALS_ver_12.90
_cell_angle_alpha                84.3098(5)
_cell_angle_beta                 89.8394(5)
_cell_angle_gamma                74.7171(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2427(1)
_cell_length_b                   18.0382(2)
_cell_length_c                   18.8848(2)
_cell_measurement_reflns_used    15546
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4001.96(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.986
_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  0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            53098
_diffrn_reflns_theta_full        25.836
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         5.115
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.34
_refine_diff_density_min         -2.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9199
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1131
_refine_ls_number_reflns         18123
_refine_ls_number_restraints     822
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.0025844
_refine_ls_shift/su_mean         5.1150661
_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: 
 12.3 15.9 7.58 2.06 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1088
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1088
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                14593
_reflns_number_total             18123
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.55
_oxford_diffrn_Wilson_scale      38.15
_oxford_refine_ls_r_factor_ref   0.0696
_oxford_refine_ls_scale          0.17619(5)
_oxford_reflns_number_all        18123
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 074ct09
_cod_data_source_file            ja1043787_si_002_11.cif
_cod_data_source_block           13
_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 '
_cod_original_formula_sum        'C80 H78 B2 F24 Ir1 N5'
_cod_database_code               4102765