Effects of Hindrance in N-Pyridyl Imidazolylidenes Coordinated to Iridium on Structure and Catalysis
Specht, Zephen G.; Grotjahn, Douglas B.; Moore, Curtis E.; Rheingold, Arnold L.; Organometallics 32 (2013) 6400–; doi:10.1021/om400758b

data_4081902
_publ_section_title
;
 Effects of Hindrance in N-Pyridyl Imidazolylidenes Coordinated to Iridium
 on Structure and Catalysis
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6400
_journal_paper_doi               10.1021/om400758b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C54 H80 Cl2 Ir2 N6, C4 H8 O2, 2(F6 P)'
_chemical_formula_sum            'C58 H88 Cl2 F12 Ir2 N6 O2 P2'
_chemical_formula_weight         1646.62
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.127(2)
_cell_angle_beta                 63.055(2)
_cell_angle_gamma                68.254(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0360(7)
_cell_length_b                   12.5925(8)
_cell_length_c                   13.0880(8)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.47
_cell_volume                     1642.46(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 1024x1024
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Photon CMOS CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26417
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  0.8154
_exptl_absorpt_correction_T_min  0.4685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.6519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                6321
_reflns_number_total             6700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400758b_si_002.cif
_cod_data_source_block           grot365
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_cell_volume        1642.46(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081902