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_7041733
_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 S Se, F6 P'
_chemical_formula_sum            'C31 H33 Cl F6 Ir N2 P S Se'
_chemical_formula_weight         917.25
_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.cc1m9vyq
_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                 91.680(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0837(16)
_cell_length_b                   19.099(4)
_cell_length_c                   22.104(4)
_cell_measurement_reflns_used    4005
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.718
_cell_measurement_theta_min      2.130
_cell_volume                     3411.2(12)
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.130
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.225
_exptl_absorpt_correction_T_max  0.4285
_exptl_absorpt_correction_T_min  0.2449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1301 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.5715.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         3.866
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5997
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0741P)^2^+53.6891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4370
_reflns_number_total             5997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04271f2.cif
_cod_data_source_block           aks04
_cod_depositor_comments
;
Adding full bibliography for 7041733--7041736.cif.

2018-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.04(C31 H33 Cl Ir N2 S Se), 0.04(F6 P)'
_cod_original_formula_sum
'C1.24 H1.32 Cl0.04 F0.24 Ir0.04 N0.08 P0.04 S0.04 Se0.04'
_cod_original_formula_units_Z    100
_cod_original_formula_weight     36.69
_cod_database_code               7041733
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9934(6) 0.0066(6)
2. 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
3. Uiso/Uaniso restraints and constraints
F5 \\sim P1 \\sim F6 \\sim F3 \\sim F4 \\sim F2 \\sim F1: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C11 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 F5, P1, F6, F3, F4, F2, F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C11, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C2(H2), C3(H3), C9(H9), C1(H1), C21(H21), C20(H20), C4(H4),
 C19(H19), C18(H18), C11(H11), C12(H12), C10(H10)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              2127
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'