Modulating reactivity in iridium bis(N-heterocyclic carbene) complexes: influence of ring size on E-H bond activation chemistry.
Phillips, Nicholas; Tang, Christina Y.; Tirfoin, Rémi; Kelly, Michael J.; Thompson, Amber L.; Gutmann, Matthias J.; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12288–12298; doi:10.1039/c4dt01398k

data_7031445
_publ_section_title
;
 Modulating reactivity in iridium bis(N-heterocyclic carbene) complexes:
 influence of ring size on E-H bond activation chemistry.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12288
_journal_page_last               12298
_journal_paper_doi               10.1039/c4dt01398k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C42 H52 Cl Ir N4'
_chemical_formula_sum            'C42 H52 Cl Ir N4'
_chemical_formula_weight         840.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-01
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 104.6968(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8693(1)
_cell_length_b                   12.3445(1)
_cell_length_c                   21.1450(2)
_cell_measurement_reflns_used    9434
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4006.75(6)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            138077
_diffrn_reflns_theta_full        26.925
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         5.130
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.431
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.50
_refine_diff_density_min         -1.43
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9099
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.0027828
_refine_ls_shift/su_mean         0.0000294
_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: 
 9.29 13.0 6.35 1.76 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0732
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0732
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7269
_reflns_number_total             9099
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      69.36
_oxford_refine_ls_r_factor_ref   0.0424
_oxford_refine_ls_scale          0.12102(2)
_oxford_reflns_number_all        9099
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 066nprt13
_cod_data_source_file            c4dt01398k1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7031443--7031451.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7031445