Synthesis, Diastereomer Separation, and Optoelectronic and Structural Properties of Dinuclear Cyclometalated Iridium(III) Complexes with Bridging Diarylhydrazide Ligands
Congrave, Daniel G.; Hsu, Yu-ting; Batsanov, Andrei S.; Beeby, Andrew; Bryce, Martin R.; Organometallics 36 (2017) 981–; doi:10.1021/acs.organomet.6b00887

data_4089194
_publ_section_title
;
 Synthesis, Diastereomer Separation, and Optoelectronic and Structural
 Properties of Dinuclear Cyclometalated Iridium(III) Complexes with
 Bridging Diarylhydrazide Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              981
_journal_paper_doi               10.1021/acs.organomet.6b00887
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety
'C58 H46 F8 Ir2 N10 O2,2(C H2 Cl2),0.5(C6 H14)'
_chemical_formula_sum            'C63 H57 Cl4 F8 Ir2 N10 O2'
_chemical_formula_weight         1664.38
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3803(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2699(6)
_cell_length_b                   28.0760(12)
_cell_length_c                   16.8768(7)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.02
_cell_measurement_theta_min      2.45
_cell_volume                     6296.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
'SHELXL 2014/7 multi-CPU version (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.110
_diffrn_source                   'I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.469
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.4085
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1069 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.4119.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.676
_refine_diff_density_min         -2.782
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         18347
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+24.7450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14811
_reflns_number_total             18347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00887_si_002.cif
_cod_data_source_block           14b-DCM-hexane
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089194
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.289
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_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. Restrained distances
 Cl2B-C59B \\sim Cl1B-C59B \\sim Cl1-C59A \\sim Cl2A-C59A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C59A) = Uiso(C59B)
Uiso(C60A) = Uiso(C60B)
4. Others
 Fixed Sof: Cl1B(0.15) Cl2B(0.15) C59B(0.15) H59C(0.15) H59D(0.15) Cl4A(0.55)
 C60A(0.55) H60A(0.55) H60B(0.55) Cl4B(0.45) C60B(0.45) H60C(0.45) H60D(0.45)
 Cl1(0.85) Cl2A(0.85) C59A(0.85) H59A(0.85) H59B(0.85)
5.a Secondary CH2 refined with riding coordinates:
 C59B(H59C,H59D), C60A(H60A,H60B), C60B(H60C,H60D), C59A(H59A,H59B), C62(H62A,
 H62B), C63(H63A,H63B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19),
 C20(H20), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
  C35(H35), C36(H36), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C53(H53), C55(H55), C56(H56), C57(H57), C58(H58)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C61(H61A,H61B,H61C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'