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_7031450
_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
'0.57(C44 H62 B Ir N5), 0.43(C44 H64 B Ir N5), C32 H12 B F24'
_chemical_formula_sum            'C76 H74.86 B2 F24 Ir N5'
_chemical_formula_weight         1728.11
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-01-22
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                88.2727(4)
_cell_angle_beta                 70.2021(5)
_cell_angle_gamma                87.5305(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7291(1)
_cell_length_b                   17.5467(2)
_cell_length_c                   18.0265(2)
_cell_measurement_reflns_used    16488
_cell_measurement_temperature    100
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3784.27(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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  0.027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66843
_diffrn_reflns_theta_full        26.393
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         5.110
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1737.713
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.80
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         17238
_refine_ls_number_restraints     652
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.0030306
_refine_ls_shift/su_mean         0.0000258
_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: 
 18.5 27.1 12.8 3.30 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1042
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1042
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                15356
_reflns_number_total             17238
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      29.58
_oxford_refine_ls_r_factor_ref   0.0486
_oxford_refine_ls_scale          0.17356(5)
_oxford_reflns_number_all        17238
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '069npmk12 (formerly 078npmk11)'
_cod_data_source_file            c4dt01398k1.cif
_cod_data_source_block           11-and-12(X-ray)
_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.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' 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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C76 H74.86 B2 F24 Ir1 N5'
_cod_database_code               7031450