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_7031447
_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         'C44 H56 Cl1 Ir1 N4'
_chemical_formula_sum            'C44 H56 Cl Ir N4'
_chemical_formula_weight         868.63
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-02-10
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.9414(5)
_cell_length_b                   21.5369(3)
_cell_length_c                   8.42331(9)
_cell_measurement_reflns_used    14970
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     7790.08(16)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            21447
_diffrn_reflns_theta_full        76.634
_diffrn_reflns_theta_max         76.634
_diffrn_reflns_theta_min         4.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.530
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.06
_refine_diff_density_min         -1.01
_refine_ls_abs_structure_details 'Flack (1983), 1331 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.038(11)
_refine_ls_extinction_coef       28(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0634
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.0006405
_refine_ls_shift/su_mean         0.0000962
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +26.61P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0571
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0571
_reflns_limit_h_max              54
_reflns_limit_h_min              0
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              -8
_reflns_number_gt                3501
_reflns_number_total             3523
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.30
_oxford_diffrn_Wilson_scale      1.56
_oxford_refine_ls_r_factor_ref   0.0211
_oxford_refine_ls_scale          0.917(3)
_oxford_reflns_number_all        3506
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 049NPMK11
_cod_data_source_file            c4dt01398k1.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/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
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7031443--7031451.cif.
;
_cod_original_cell_volume        7790.10(15)
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_original_formula_sum        'C44 H56 Cl1 Ir1 N4'
_cod_database_code               7031447