Mono and dimetallic pyrene-imidazolylidene complexes of iridium(iii) for the deuteration of organic substrates and the C-C coupling of alcohols.
Ibañez, S; Poyatos, M.; Peris, E.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14154–14159; doi:10.1039/c6dt02942f

data_7040161
_publ_section_title
;
 Mono and dimetallic pyrene-imidazolylidene complexes of iridium(iii) for
 the deuteration of organic substrates and the C-C coupling of alcohols.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14154
_journal_page_last               14159
_journal_paper_doi               10.1039/c6dt02942f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C38 H45 Ir N2 O3, 2(C H Cl3)'
_chemical_formula_sum            'C40 H47 Cl6 Ir N2 O3'
_chemical_formula_weight         1008.69
_chemical_name_systematic        SI538K3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3211(6)
_cell_length_b                   24.2943(9)
_cell_length_c                   12.1511(4)
_cell_measurement_reflns_used    7803
_cell_measurement_temperature    160.3(9)
_cell_measurement_theta_max      28.9410
_cell_measurement_theta_min      2.9430
_cell_volume                     4227.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.3(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -26.00  55.90   0.70    8.00    --  -10.50  57.00   0.00  117
  2  \w     28.00  53.90   0.70    8.00    --   11.52 -99.00 120.00   37
  3  \w    -20.00   8.00   0.70    8.00    --   11.52 -99.00 120.00   40
  4  \w     -3.00  49.50   0.70    8.00    --   11.52 -99.00  30.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0406016000
_diffrn_orient_matrix_UB_12      0.0145088000
_diffrn_orient_matrix_UB_13      -0.0167144000
_diffrn_orient_matrix_UB_21      0.0180076000
_diffrn_orient_matrix_UB_22      0.0244401000
_diffrn_orient_matrix_UB_23      0.0236439000
_diffrn_orient_matrix_UB_31      0.0219455000
_diffrn_orient_matrix_UB_32      0.0066513000
_diffrn_orient_matrix_UB_33      -0.0506845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and chloroform'
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.219
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+20.8870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3926
_reflns_number_total             4410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02942f2.cif
_cod_data_source_block           str1854
_cod_depositor_comments
'Adding full bibliography for 7040159--7040161.cif.'
_cod_database_code               7040161
_chemical_oxdiff_formula         'C38 H45 N2 O3 Ir'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Others
 Fixed Sof: H25C(0.5) H25B(0.5) H25A(0.5)
3.a Ternary CH refined with riding coordinates:
 C22(H138)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H45), C9(H58), C5(H61)
3.c Idealised Me refined as rotating group:
 C13(H7A,H7B,H7C), C2(H43A,H43B,H43C), C14(H11A,H11B,H11C), C20(H12A,H12B,
 H12C), C12(H15A,H15B,H15C), C19(H16A,H16B,H16C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.893