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_4089199
_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         'C62 H38 F12 Ir2 N6 O2, 2(C D2 Cl2)'
_chemical_formula_sum            'C64 H38 Cl4 D4 F12 Ir2 N6 O2'
_chemical_formula_weight         1685.26
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                64.1255(12)
_cell_angle_beta                 63.4417(12)
_cell_angle_gamma                84.4419(13)
_cell_formula_units_Z            1
_cell_length_a                   11.6609(5)
_cell_length_b                   12.6394(5)
_cell_length_c                   12.6537(6)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    120
_cell_measurement_theta_max      35.58
_cell_measurement_theta_min      3.15
_cell_volume                     1489.73(11)
_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_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40288
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.577
_diffrn_reflns_theta_min         2.080
_diffrn_source                   'I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.731
_exptl_absorpt_correction_T_max  0.5571
_exptl_absorpt_correction_T_min  0.3019
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0965 before and 0.0386 after correction.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00246(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         12509
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0148
_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^)+(0.0130P)^2^+0.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0350
_refine_ls_wR_factor_ref         0.0356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11958
_reflns_number_total             12509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00887_si_002.cif
_cod_data_source_block           16a-2dDCM
_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               4089199
_shelx_estimated_absorpt_t_max   0.545
_shelx_estimated_absorpt_t_min   0.243
_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
 F3A-C9 \\sim F3B-C9 \\sim F4B-C9 \\sim F5A-C9 \\sim F5B-C9 \\sim F4A-C9 \\sim
F3C-C9 \\sim F3C-C9 \\sim F4C-C9
 with sigma of 0.02
 F3A-F4A \\sim F3A-F5A \\sim F4A-F5A \\sim F3B-F4B \\sim F3B-F5B \\sim F4B-F5B
\\sim F3C-F4C \\sim F3C-F5C
 \\sim F4C-F5C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5B) = Uanis(F4C)
Uanis(F3C) = Uanis(F4B)
Uanis(F3B) = Uanis(F5C)
4. Others
 Fixed Sof: F5A(0.75) F4A(0.75) F3A(0.75) F3B(0.1) F4B(0.1) F5B(0.1) Cl1A(0.5)
 Cl2A(0.42) C2A(0.5) D2AA(0.5) D2AB(0.5) Cl2C(0.08) Cl1B(0.5) Cl2B(0.5)
 C2B(0.5) D2BA(0.5) D2BB(0.5) F3C(0.15) F4C(0.15) F5C(0.15)
5.a Secondary CH2 refined with riding coordinates:
 C2A(D2AA,D2AB), C2B(D2BA,D2BB)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'