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_7031443
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 H46 Ir1 N4'
_chemical_formula_sum            'C40 H46 Ir N4'
_chemical_formula_weight         775.05
_chemical_melting_point          ?
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-05-02
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 94.9522(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0172(3)
_cell_length_b                   15.0295(6)
_cell_length_c                   12.2995(5)
_cell_measurement_reflns_used    3727
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1660.66(11)
_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 0.990
_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  0.090
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15631
_diffrn_reflns_theta_full        26.939
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         5.149
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.055
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.96
_refine_diff_density_min         -5.76
_refine_ls_abs_structure_details 'Flack (1983), 7051 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.437(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.0003711
_refine_ls_shift/su_mean         0.0000168
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 4.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0946
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0946
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5113
_reflns_number_total             7051
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      82.33
_oxford_refine_ls_r_factor_ref   0.0877
_oxford_refine_ls_scale          0.11261(3)
_oxford_reflns_number_all        7050
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 045np12
_cod_data_source_file            c4dt01398k1.cif
_cod_data_source_block           1-prime
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031443--7031451.cif.

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 1 '
_cod_original_formula_sum        'C40 H46 Ir1 N4'
_cod_database_code               7031443