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_4079745
_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         'C32 H12 B F24, C44 H58 Ir N4'
_chemical_formula_sum            'C76 H70 B F24 Ir N4'
_chemical_formula_weight         1698.40
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-08-22
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                91.7424(4)
_cell_angle_beta                 110.8926(4)
_cell_angle_gamma                90.7674(7)
_cell_formula_units_Z            2
_cell_length_a                   13.83290(10)
_cell_length_b                   16.2697(2)
_cell_length_c                   17.7359(2)
_cell_measurement_reflns_used    14915
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3726.17(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 0.989
_diffrn_measured_fraction_theta_max 0.985
_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  0.024
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51811
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         5.120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.63
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8450
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         16839
_refine_ls_number_restraints     486
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.0045178
_refine_ls_shift/su_mean         0.0000622
_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: 
 23.4 33.2 16.5 4.36 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1077
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1077
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                14550
_reflns_number_total             16839
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      21.43
_oxford_refine_ls_r_factor_ref   0.0533
_oxford_refine_ls_scale          0.22649(9)
_oxford_reflns_number_all        16839
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 022np11
_cod_data_source_file            om301060h_si_002.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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      'P -1 '
_cod_original_formula_sum        'C76 H70 B1 F24 Ir1 N4'
_cod_database_code               4079745
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
RIDE IR  (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,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   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) H   ( 433,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(52) F(300) F(301) F(302) AND 
CONT C(52) F(301) F(302) F(300) AND 
CONT C(52) F(302) F(300) F(301) AND 
CONT C(52) F(303) F(304) F(305) AND 
CONT C(52) F(304) F(305) F(303) AND 
CONT C(52) F(305) F(303) F(304) 
SIMU 0.01  C(52) F(300) F(301) F(302) AND 
CONT C(52) F(301) F(302) F(300) AND 
CONT C(52) F(302) F(300) F(301) AND 
CONT C(52) F(303) F(304) F(305) AND 
CONT C(52) F(304) F(305) F(303) AND 
CONT C(52) F(305) F(303) F(304) 
DELU 0.01  C(52) F(300) F(301) F(302) AND 
CONT C(52) F(301) F(302) F(300) AND 
CONT C(52) F(302) F(300) F(301) AND 
CONT C(52) F(303) F(304) F(305) AND 
CONT C(52) F(304) F(305) F(303) AND 
CONT C(52) F(305) F(303) F(304) 
SAME C(102) F(400) F(401) F(402) AND 
CONT C(102) F(401) F(402) F(400) AND 
CONT C(102) F(402) F(400) F(401) AND 
CONT C(102) F(403) F(404) F(405) AND 
CONT C(102) F(404) F(405) F(403) AND 
CONT C(102) F(405) F(403) F(404) 
SIMU 0.01  C(102) F(400) F(401) F(402) AND 
CONT C(102) F(401) F(402) F(400) AND 
CONT C(102) F(402) F(400) F(401) AND 
CONT C(102) F(403) F(404) F(405) AND 
CONT C(102) F(404) F(405) F(403) AND 
CONT C(102) F(405) F(403) F(404) 
DELU 0.01  C(102) F(400) F(401) F(402) AND 
CONT C(102) F(401) F(402) F(400) AND 
CONT C(102) F(402) F(400) F(401) AND 
CONT C(102) F(403) F(404) F(405) AND 
CONT C(102) F(404) F(405) F(403) AND 
CONT C(102) F(405) F(403) F(404) 
SAME C(109) F(500) F(501) F(502) AND 
CONT C(109) F(501) F(502) F(500) AND 
CONT C(109) F(502) F(500) F(501) AND 
CONT C(109) F(503) F(504) F(505) AND 
CONT C(109) F(504) F(505) F(503) AND 
CONT C(109) F(505) F(503) F(504) 
SIMU 0.01  C(109) F(500) F(501) F(502) AND 
CONT C(109) F(501) F(502) F(500) AND 
CONT C(109) F(502) F(500) F(501) AND 
CONT C(109) F(503) F(504) F(505) AND 
CONT C(109) F(504) F(505) F(503) AND 
CONT C(109) F(505) F(503) F(504) 
DELU 0.01  C(109) F(500) F(501) F(502) AND 
CONT C(109) F(501) F(502) F(500) AND 
CONT C(109) F(502) F(500) F(501) AND 
CONT C(109) F(503) F(504) F(505) AND 
CONT C(109) F(504) F(505) F(503) AND 
CONT C(109) F(505) F(503) F(504) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;