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_7106025
_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         'C81 H114 Cl3 Ir3 N6'
_chemical_formula_sum            'C81 H114 Cl3 Ir3 N6'
_chemical_formula_weight         1854.85
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-10-22
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 98.7771(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.04520(10)
_cell_length_b                   12.77400(10)
_cell_length_c                   32.1598(2)
_cell_measurement_reflns_used    19648
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8544.32(9)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_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  0.060
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19421
_diffrn_reflns_theta_full        26.665
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         5.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.796
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            deep_red
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.36
_refine_diff_density_min         -0.77
_refine_ls_extinction_coef       38.135
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0550
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         10554
_refine_ls_number_restraints     540
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.0285410
_refine_ls_shift/su_mean         1.9883391
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 6.03P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0784
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0664
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                12063
_reflns_number_total             19421
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.63
_oxford_diffrn_Wilson_scale      750.83
_oxford_refine_ls_r_factor_ref   0.0316
_oxford_refine_ls_scale          0.046896(3)
_oxford_reflns_number_all        19421
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title '3052018 006ct09'
_cod_data_source_file            C0CC05431C.TXT
_cod_data_source_block           2
_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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7106025