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_4089196
_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
'C70 H62 F4 Ir2 N6 O6, 0.16(C H2 Cl2), 1.84(C H4 O)'
_chemical_formula_sum            'C72 H69.68 Cl0.32 F4 Ir2 N6 O7.84'
_chemical_formula_weight         1616.20
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-25
_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                 93.8546(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9490(4)
_cell_length_b                   13.1839(5)
_cell_length_c                   20.4762(8)
_cell_measurement_reflns_used    9546
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.68
_cell_measurement_theta_min      2.46
_cell_volume                     3218.4(2)
_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 (Sheldrick, 2015)'
_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  '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  0.0738
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            145432
_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         33.676
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.217
_exptl_absorpt_correction_T_max  0.6730
_exptl_absorpt_correction_T_min  0.4746
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.7052.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.832
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         12793
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+1.6700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10184
_reflns_number_total             12793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00887_si_002.cif
_cod_data_source_block           15a-MeOH
_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               4089196
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.471
_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
2. Restrained distances
 Cl2-C37 = Cl1-C37
 1.73 with sigma of 0.02
 Cl1-C37 \\sim Cl2-C37
 with sigma of 0.02
3. Others
 Uiso(H13A)=Uiso(H13B)=Uiso(H13C)=FVAR(1)
 Uiso(H25A)=Uiso(H25B)=Uiso(H25C)=FVAR(2)
 Uiso(H33A)=Uiso(H33B)=Uiso(H33C)=FVAR(3)
 Uiso(H34A)=Uiso(H34B)=Uiso(H34C)=FVAR(4)
 Uiso(H35A)=Uiso(H35B)=Uiso(H35C)=FVAR(5)
 Uiso(H36A)=Uiso(H36B)=Uiso(H36C)=FVAR(6)
 Fixed Sof: Cl1(0.08) Cl2(0.08) C37(0.08) H37A(0.08) H37B(0.08) O4(0.92)
 H4(0.92) C36(0.92) H36A(0.92) H36B(0.92) H36C(0.92)
4.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C17(H17),
 C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C30(H30), C31(H31)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'