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_7040159
_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         'C37 H45 Cl2 Ir N2, C7'
_chemical_formula_sum            'C44 H45 Cl2 Ir N2'
_chemical_formula_weight         864.92
_chemical_name_systematic        MP873
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     iterative
_audit_creation_date             2016-07-18
_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                 96.611(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4266(3)
_cell_length_b                   21.9900(7)
_cell_length_c                   16.1613(5)
_cell_measurement_reflns_used    13348
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.1230
_cell_measurement_theta_min      3.4450
_cell_volume                     4033.9(2)
_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(2)
_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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -14.00  88.20   0.70   25.00    --   11.59  37.00-180.00  146
  2  \w     34.00 100.50   0.70   25.00    --   11.59-178.00  90.00   95
  3  \w    -67.00  45.00   0.70   25.00    --   11.59 -77.00-120.00  160
  4  \w    -22.00  49.40   0.70   25.00    --   11.59  77.00 -60.00  102
;
_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      -0.0242644000
_diffrn_orient_matrix_UB_12      0.0188759000
_diffrn_orient_matrix_UB_13      -0.0332327000
_diffrn_orient_matrix_UB_21      -0.0398094000
_diffrn_orient_matrix_UB_22      0.0125119000
_diffrn_orient_matrix_UB_23      0.0259818000
_diffrn_orient_matrix_UB_31      0.0415923000
_diffrn_orient_matrix_UB_32      0.0229773000
_diffrn_orient_matrix_UB_33      0.0131476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and chloroform'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8223
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0362P)^2^+17.7085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7001
_reflns_number_total             8223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02942f2.cif
_cod_data_source_block           str1852
_cod_depositor_comments
'Adding full bibliography for 7040159--7040161.cif.'
_cod_database_code               7040159
_chemical_oxdiff_formula         'C37 H45 N2 Cl2 Ir'
_reflns_odcompleteness_completeness 99.76
_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. Restrained distances
 C43-C42 \\sim C41-C40 \\sim C39-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
6.a Free rotating group:
 C44(C39,C43,C14A,C13A,C12A,C38,C42,C40,C41)
6.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C10(H10), C27(H27), C24(H24), C5(H5), C9(H9)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C2(H2A,H2B,H2C), C36(H36A,H36B,H36C), C32(H32A,H32B,
 H32C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C13A(H13D,H13E,
 H13F), C12A(H12D,H12E,H12F)
;
_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 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.843