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_7031451
_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
'0.65(C44 H62 B Ir N5), 0.35(C44 H64 B Ir N5), C32 H12 B F24'
_chemical_formula_sum            'C76 H74.7 B2 F24 Ir N5'
_chemical_formula_weight         1727.96
_chemical_melting_point          ?
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.275(19)
_cell_angle_beta                 70.175(17)
_cell_angle_gamma                87.82(2)
_cell_formula_units_Z            2
_cell_length_a                   12.689(3)
_cell_length_b                   17.5549(16)
_cell_length_c                   17.948(4)
_cell_measurement_reflns_used    1100
_cell_measurement_temperature    100(2)
_cell_volume                     3757.7(13)
_computing_cell_refinement       SXD2001
_computing_data_collection       SXD2001
_computing_data_reduction        SXD2001
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Refinement of known model'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.027
_diffrn_measured_fraction_theta_max 0.027
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     Laue
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1570
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7639
_diffrn_reflns_theta_full        84.73
_diffrn_reflns_theta_max         84.73
_diffrn_reflns_theta_min         9.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    '3.59353 + 0.589577 * lambda'
_exptl_absorpt_correction_T_max  0.7174
_exptl_absorpt_correction_T_min  0.4149
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Calculated using custom ISIS software program SXD-2001.
;
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             859
_exptl_crystal_size_max          6.0
_exptl_crystal_size_mid          3.0
_exptl_crystal_size_min          2.0
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.000536(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1480
_refine_ls_number_reflns         7639
_refine_ls_number_restraints     4446
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                6529
_reflns_number_total             7639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01398k1.cif
_cod_data_source_block           11-and-12(Neutron)
_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.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' 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.

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_cell_volume        3757.7(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C76 H74.70 B2 F24 Ir N5'
_cod_database_code               7031451