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_7040160
_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         'C26 H32 Ir N2 O3, 3(C H Cl3)'
_chemical_formula_sum            'C29 H35 Cl9 Ir N2 O3'
_chemical_formula_weight         970.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-22 deposited with the CCDC.
2016-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.986(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2410(5)
_cell_length_b                   21.8290(9)
_cell_length_c                   13.3907(5)
_cell_measurement_reflns_used    14129
_cell_measurement_temperature    200.0(4)
_cell_measurement_theta_max      28.8990
_cell_measurement_theta_min      4.2050
_cell_volume                     3720.7(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      200.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -20.00  31.60   0.60   30.00    --  -10.50 -99.00  60.00   86
  2  \w    -86.00 -37.40   0.60   30.00    --  -10.50 153.00 -66.59   81
  3  \w    -20.00  31.60   0.60   30.00    --  -10.50 -99.00-120.00   86
  4  \w    -35.00  92.80   0.60   30.00    --   11.52  19.00  30.00  213
  5  \w    -44.00  68.80   0.60   30.00    --  -10.50  77.00-120.00  188
  6  \w    -15.00  14.40   0.60   30.00    --   11.52  37.00-120.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0049047000
_diffrn_orient_matrix_UB_12      0.0318660000
_diffrn_orient_matrix_UB_13      0.0107375000
_diffrn_orient_matrix_UB_21      0.0401948000
_diffrn_orient_matrix_UB_22      0.0019434000
_diffrn_orient_matrix_UB_23      -0.0256078000
_diffrn_orient_matrix_UB_31      -0.0382612000
_diffrn_orient_matrix_UB_32      0.0061329000
_diffrn_orient_matrix_UB_33      -0.0475658000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.267
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.908
_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    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             1908
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and chloroform'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0380P)^2^+11.7980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6689
_reflns_number_total             7581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02942f2.cif
_cod_data_source_block           str1859
_cod_depositor_comments
'Adding full bibliography for 7040159--7040161.cif.'
_cod_original_cell_volume        3720.8(3)
_cod_database_code               7040160
_chemical_oxdiff_formula         C52H64N4O6Ir2
_reflns_odcompleteness_completeness 99.71
_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,H) groups
2.a Ternary CH refined with riding coordinates:
 C32(H85), C31(H123), C30(H125)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H77), C6(H90)
2.c Idealised Me refined as rotating group:
 C27(H8A,H8B,H8C), C24(H26A,H26B,H26C), C17(H59A,H59B,H59C), C3(H92A,H92B,
 H92C), C16(H97A,H97B,H97C), C2(H10A,H10B,H10C), C15(H12A,H12B,H12C), C23(H13A,
 H13B,H13C), C25(H13D,H13E,H13F), C26(H1A,H1B,H1C)
;
_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.822