Complexes of (η(5)-Cp*)Ir(iii) with 1-benzyl-3-phenylthio/selenomethyl-1,3-dihydrobenzoimidazole-2-thione/selenone: catalyst for oxidation and 1,2-substituted benzimidazole synthesis.
Sharma, Alpesh K.; Joshi, Hemant; Bhaskar, Renu; Singh, Ajai K.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2228–2237; doi:10.1039/c6dt04271f

data_7041736
_publ_section_title
;
 Complexes of (\h(5)-Cp*)Ir(iii) with
 1-benzyl-3-phenylthio/selenomethyl-1,3-dihydrobenzoimidazole-2-thione/selenone:
 catalyst for oxidation and 1,2-substituted benzimidazole synthesis.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2228
_journal_page_last               2237
_journal_paper_doi               10.1039/c6dt04271f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C31 H33 Cl Ir N2 S2, F6 P'
_chemical_formula_sum            'C31 H33 Cl F6 Ir N2 P S2'
_chemical_formula_weight         870.33
_chemical_name_systematic
;
 ? 
;
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1lhh9w
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-26 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.279(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0195(14)
_cell_length_b                   19.158(3)
_cell_length_c                   22.138(4)
_cell_measurement_reflns_used    7107
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.313
_cell_measurement_theta_min      2.317
_cell_volume                     3400.4(10)
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40117
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.406
_exptl_absorpt_coefficient_mu    4.232
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1484 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.6670.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.772
_refine_diff_density_min         -2.239
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+6.4289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5094
_reflns_number_total             6000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04271f2.cif
_cod_data_source_block           aks88m
_cod_depositor_comments
'Adding full bibliography for 7041733--7041736.cif.'
_cod_database_code               7041736
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C3(H3), C1(H1), C21(H21), C2(H2), C20(H20), C18(H18), C17(H17),
 C5(H5), C9(H9), C19(H19), C4(H4), C10(H10), C11(H11)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              13359
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'