Sterically Encumbered Iridium Bis(N-heterocyclic carbene) Complexes: Air-Stable 14-Electron Cations and Facile Degenerate C‒H Activation
Phillips, Nicholas; Rowles, Johnny; Kelly, Michael J.; Riddlestone, Ian; Rees, Nicholas H.; Dervisi, Athanasia; Fallis, Ian A.; Aldridge, Simon; Organometallics 31 (2012) 8075–; doi:10.1021/om301060h

data_4079742
_publ_section_title
;
 Sterically Encumbered Iridium Bis(N-heterocyclic carbene) Complexes:
 Air-Stable 14-Electron Cations and Facile Degenerate C--H Activation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8075
_journal_paper_doi               10.1021/om301060h
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C46 H59 Ir1 N4'
_chemical_formula_sum            'C46 H59 Ir N4'
_chemical_formula_weight         860.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             12-08-22
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 120.2697(6)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.1355(4)
_cell_length_b                   20.8001(3)
_cell_length_c                   20.6871(3)
_cell_measurement_reflns_used    13116
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     11942.5(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55182
_diffrn_reflns_theta_full        25.279
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         5.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.391
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         6.37
_refine_diff_density_min         -5.38
_refine_ls_extinction_coef       160(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         13541
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0007090
_refine_ls_shift/su_mean         0.0000139
_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: 
 1.68 0.882 0.122 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1022
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.1022
_reflns_limit_h_max              35
_reflns_limit_h_min              -41
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                8280
_reflns_number_total             13541
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.56
_oxford_diffrn_Wilson_scale      823.22
_oxford_refine_ls_r_factor_ref   0.1077
_oxford_refine_ls_scale          0.0214073(13)
_oxford_reflns_number_all        13541
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 295npct10
_cod_data_source_file            om301060h_si_002.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C46 H59 Ir1 N4'
_cod_database_code               4079742
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE IR  (   1,X'S) H   (  11,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  63,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 113,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 123,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 253,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 263,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) H   ( 313,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 372,X'S) H   ( 371,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 502,X'S) H   ( 501,X'S) H   ( 503,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 511,X'S) H   ( 513,X'S) 
RIDE IR  (  52,X'S) H   ( 521,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 582,X'S) H   ( 581,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,X'S) H   ( 673,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) H   ( 683,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 752,X'S) H   ( 753,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 763,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 773,X'S) H   ( 772,X'S) H   ( 771,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;