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_7106029
_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         'C54 H76 Ir2 N4, 2(C32 H12 B F24)'
_chemical_formula_sum            'C118 H100 B2 F48 Ir2 N4'
_chemical_formula_weight         2892.08
_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             10-11-22
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                76.3183(8)
_cell_angle_beta                 78.8084(8)
_cell_angle_gamma                88.2739(8)
_cell_formula_units_Z            1
_cell_length_a                   13.7443(2)
_cell_length_b                   14.4652(3)
_cell_length_c                   15.3265(3)
_cell_measurement_reflns_used    9501
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     2903.96(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 0.989
_diffrn_measured_fraction_theta_max 0.986
_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  0.050
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28572
_diffrn_reflns_theta_full        25.232
_diffrn_reflns_theta_max         26.012
_diffrn_reflns_theta_min         5.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_orange
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.54
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9959
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         9955
_refine_ls_number_restraints     2166
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.0085655
_refine_ls_shift/su_mean         0.0001949
_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:
13.6 18.5 8.79 2.31
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1225
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1225
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                8396
_reflns_number_total             11260
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.48
_oxford_diffrn_Wilson_scale      85.17
_oxford_refine_ls_r_factor_ref   0.0639
_oxford_refine_ls_scale          0.18157(10)
_oxford_reflns_number_all        9955
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 229ct10
_cod_data_source_file            C0CC05431C.TXT
_cod_data_source_block           229ct10
_cod_depositor_comments
;
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_database_code               7106029