Responses to unsaturation in iridium mono(N-heterocyclic carbene) complexes: synthesis and oligomerization of [LIr(H)2Cl] and [LIr(H)2]+
Christina Y. Tang; Jan Lednik; Dragoslav Vidovic; Amber L. Thompson; Simon Aldridge; Chem.Commun. 47 (2011) 2523–; doi:10.1039/c0cc05431c

data_7106031
_publ_section_title
;
 Responses to unsaturation in iridium mono(N-heterocyclic carbene)
 complexes: synthesis and oligomerization of [LIr(H)2Cl] and [LIr(H)2]+
;
_journal_name_full               Chem.Commun.
_journal_page_first              2523
_journal_paper_doi               10.1039/c0cc05431c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C58 H72 Cl Ir2 N4, C32 H12 B F24'
_chemical_formula_sum            'C90 H84 B Cl F24 Ir2 N4'
_chemical_formula_weight         2108.34
_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
_audit_creation_date             10-10-25
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                94.97(3)
_cell_angle_beta                 110.90(3)
_cell_angle_gamma                94.15(3)
_cell_formula_units_Z            2
_cell_length_a                   15.333(3)
_cell_length_b                   15.589(3)
_cell_length_c                   19.855(4)
_cell_measurement_reflns_used    17645
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4389.7(18)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_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  0.030
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71291
_diffrn_reflns_theta_full        25.270
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         5.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.157
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.06
_refine_diff_density_min         -3.36
_refine_ls_extinction_coef       96.533
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9087
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1320
_refine_ls_number_reflns         19837
_refine_ls_number_restraints     1204
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.0130284
_refine_ls_shift/su_mean         0.4666595
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +27.63P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1206
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1205
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                13842
_reflns_number_total             19838
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0837
_oxford_refine_ls_scale          0.15306(4)
_oxford_reflns_number_all        19838
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 076ct09
_cod_data_source_file            C0CC05431C.TXT
_cod_data_source_block           8
_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 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4389.4(18)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C90 H84 B1 Cl1 F24 Ir2 N4'
_cod_database_code               7106031