Sterically hindered phenanthroimidazole ligands drive the structural flexibility and facile ligand exchange in cyclometalated iridium(III) complexes.
Tatarin, Sergei V.; Kalle, Paulina; Taydakov, Ilya V.; Varaksina, Evgenia A.; Korshunov, Vladislav M.; Bezzubov, Stanislav I.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6889–6900; doi:10.1039/d1dt00820j

data_7707210
_publ_section_title
;
 Sterically hindered phenanthroimidazole ligands drive the structural
 flexibility and facile ligand exchange in cyclometalated iridium(III)
 complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6889
_journal_page_last               6900
_journal_paper_doi               10.1039/d1dt00820j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '0.5(C122 H76 Ir2 N8 O4 S), 0.5(C2 H3 N)'
_chemical_formula_sum            'C62 H39.5 Ir N4.5 O2 S0.5'
_chemical_formula_weight         1087.71
_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     iterative
_audit_creation_date             2020-12-23
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-12-23 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                111.7180(10)
_cell_angle_beta                 97.9180(10)
_cell_angle_gamma                105.2410(10)
_cell_formula_units_Z            4
_cell_length_a                   13.7602(5)
_cell_length_b                   18.4965(5)
_cell_length_c                   22.4727(6)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.22
_cell_volume                     4947.4(3)
_computing_cell_refinement       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54309
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         2.003
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.770
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0556 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8801.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN, CDCl3'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1373
_refine_ls_number_reflns         20035
_refine_ls_number_restraints     556
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0372P)^2^+4.9674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15658
_reflns_number_total             20035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00820j2.cif
_cod_data_source_block           st35h
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707205--7707218.cif.
;
_cod_original_formula_sum        'C62 H39.50 Ir N4.50 O2 S0.50'
_cod_database_code               7707210
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.666
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C135-C61 \\sim C62-C61
 with sigma of 0.02
 C57-C58 \\sim C143-C58
 with sigma of 0.02
 C126-C48 \\sim C47-C48
 with sigma of 0.02
 N8-C103 \\sim N8-C139
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C126 \\sim C127 \\sim C130 \\sim C131 \\sim C129 \\sim C128 \\sim C47 \\sim C42
\\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C67 \\sim C66
\\sim C62 \\sim C65 \\sim C63 \\sim C64: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C139 \\sim C140 \\sim C141 \\sim C142 \\sim C144 \\sim C145 \\sim C103 \\sim
C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) = Uanis(C146) = Uanis(C0) = Uanis(C132) = Uanis(C24) = Uanis(C23) =
Uanis(C22) = Uanis(C123) = Uanis(C26) = Uanis(C21) = Uanis(C124) = Uanis(C125)
Uiso(H143) = Uiso(H57)
4. Others
 Fixed Sof: S1(0.6) S005(0.4) C26(0.6) C25(0.6) H25(0.6) C24(0.6) H24(0.6)
 C23(0.6) H23(0.6) C22(0.6) H22(0.6) C21(0.6) C139(0.35) C141(0.35) H141(0.35)
 C145(0.35) H145(0.35) C144(0.35) H144(0.35) C142(0.35) H142(0.35) C140(0.35)
 H140(0.35) C134(0.4) C136(0.4) H136(0.4) C138(0.4) H138(0.4) C137(0.4)
 H137(0.4) C135(0.4) C133(0.4) H133(0.4) C126(0.5) C127(0.5) C130(0.5)
 H130(0.5) C131(0.5) H131(0.5) C129(0.5) H129(0.5) C128(0.5) H128(0.5)
 C146(0.4) H146(0.4) C125(0.4) C124(0.4) C123(0.4) H123(0.4) C0(0.4) H0(0.4)
 C132(0.4) H132(0.4) C57(0.6) C143(0.4) C47(0.5) C42(0.5) C43(0.5) H43(0.5)
 C44(0.5) H44(0.5) C45(0.5) H45(0.5) C46(0.5) H46(0.5) C67(0.6) H67(0.6)
 C66(0.6) C62(0.6) C65(0.6) H65(0.6) C63(0.6) H63(0.6) C64(0.6) H64(0.6)
 C103(0.65) C104(0.65) H104(0.65) C108(0.65) H108(0.65) C105(0.65) H105(0.65)
 C106(0.65) H106(0.65) C107(0.65) H107(0.65) H57(0.6) H143(0.4)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C87(H87), C81(H81), C84(H84), C73(H73), C93(H93), C97(H97), C5(H5),
 C92(H92), C25(H25), C24(H24), C23(H23), C22(H22), C32(H32), C77(H77), C85(H85),
  C114(H114), C12(H12), C100(H100), C79(H79), C9(H9), C86(H86), C141(H141),
 C145(H145), C144(H144), C142(H142), C140(H140), C78(H78), C16(H16), C80(H80),
 C4(H4), C113(H113), C18(H18), C98(H98), C30(H30), C136(H136), C138(H138),
 C137(H137), C133(H133), C31(H31), C111(H111), C3(H3), C29(H29), C51(H51),
 C91(H91), C60(H60), C70(H70), C112(H112), C10(H10), C72(H72), C13(H13),
 C90(H90), C71(H71), C19(H19), C52(H52), C2(H2), C36(H36), C120(H120),
 C117(H117), C17(H17), C50(H50), C118(H118), C49(H49), C119(H119), C37(H37),
 C99(H99), C40(H40), C38(H38), C130(H130), C131(H131), C129(H129), C128(H128),
 C146(H146), C123(H123), C0(H0), C132(H132), C39(H39), C43(H43), C44(H44),
 C45(H45), C46(H46), C67(H67), C65(H65), C63(H63), C64(H64), C104(H104),
 C108(H108), C105(H105), C106(H106), C107(H107)
5.b Fitted hexagon refined as free rotating group:
 C26(C25,C24,C23,C22,C21), C139(C141,C145,C144,C142,C140), C134(C136,C138,C137,
 C135,C133), C126(C127,C130,C131,C129,C128), C146(C125,C124,C123,C0,C132),
 C47(C42,C43,C44,C45,C46)
5.c Idealised Me refined as rotating group:
 C03H(H03A,H03B,H03C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37332
_shelx_hkl_checksum              5202
_shelx_fab_checksum              29988
_olex2_submission_special_instructions 'No special instructions were received'