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_7106028
_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         'C33 H43 F Ir N2, C32 H12 B F24'
_chemical_formula_sum            'C65 H55 B F25 Ir N2'
_chemical_formula_weight         1542.15
_chemical_melting_point          ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-11-02
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.75620(10)
_cell_length_b                   25.43320(10)
_cell_length_c                   53.9834(3)
_cell_measurement_reflns_used    26847
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     25751.7(2)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.955
_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  0.037
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            135985
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12256
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.61
_refine_diff_density_min         -3.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9412
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2075
_refine_ls_number_reflns         28196
_refine_ls_number_restraints     2140
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.0477654
_refine_ls_shift/su_mean         4.1479988
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +*****P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1733
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1733
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              70
_reflns_limit_l_min              0
_reflns_number_gt                18631
_reflns_number_total             28197
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.93
_oxford_diffrn_Wilson_scale      363.67
_oxford_refine_ls_r_factor_ref   0.1052
_oxford_refine_ls_scale          0.054083(6)
_oxford_reflns_number_all        28197
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 139ct10
_cod_data_source_file            C0CC05431C.TXT
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C65 H55 B1 F25 Ir1 N2'
_cod_database_code               7106028