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_4089193
_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, C H2 Cl2'
_chemical_formula_sum            'C59 H48 Cl2 F8 Ir2 N10 O2'
_chemical_formula_weight         1536.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                101.874(2)
_cell_angle_beta                 90.127(2)
_cell_angle_gamma                111.257(2)
_cell_formula_units_Z            4
_cell_length_a                   12.8729(8)
_cell_length_b                   17.6403(11)
_cell_length_c                   27.5904(17)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.47
_cell_volume                     5693.8(6)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker 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  0.0435
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            112010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.274
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.843
_exptl_absorpt_correction_T_max  0.5435
_exptl_absorpt_correction_T_min  0.4472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.8228.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.143
_refine_diff_density_max         3.828
_refine_diff_density_min         -3.252
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1496
_refine_ls_number_reflns         43598
_refine_ls_number_restraints     1596
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+4.3030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33829
_reflns_number_total             43598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00887_si_002.cif
_cod_data_source_block           14b-metastable
_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               4089193
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.394
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9439(2) 0.0561(2)
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. 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
4.a Riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C9'(H9'A,H9'B,H9'C),
 C10'(H10D,H10E,H10F), C11'(H11D,H11E,H11F), C38'(H38D,H38E,H38F), C39'(H39D,
 H39E,H39F), C40'(H40D,H40E,H40F)
4.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B)
4.c 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), 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')
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'