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_7707215
_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         'C122 H72 Cl4 Ir2 N8 O4 S, 2(C2 H3 N)'
_chemical_formula_sum            'C126 H78 Cl4 Ir2 N10 O4 S'
_chemical_formula_weight         2354.24
_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
_audit_creation_date             2021-03-10
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-03-10 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.336(8)
_cell_angle_beta                 101.460(9)
_cell_angle_gamma                102.695(8)
_cell_formula_units_Z            2
_cell_length_a                   12.202(3)
_cell_length_b                   20.438(5)
_cell_length_c                   21.092(6)
_cell_measurement_reflns_used    3632
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      2.36
_cell_volume                     4911(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1744
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.287
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1050 before and 0.0808 after correction.
The Ratio of minimum to maximum transmission is 0.7884.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       needle
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         17415
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10170
_reflns_number_total             17415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00820j2.cif
_cod_data_source_block           st37h
_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_database_code               7707215
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.594
_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
 N00H-C1E \\sim N00H-C20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim C1G: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C1G) = Uanis(C23) = Uanis(C25) = Uanis(C24) = Uanis(C1F) = Uanis(C21) =
Uanis(C1E) = Uanis(C22) = Uanis(C1H) = Uanis(C1J) = Uanis(C1I)
Uanis(C0) = Uanis(C2) = Uanis(C5) = Uanis(C3) = Uanis(C4) = Uanis(C7) =
Uanis(C6) = Uanis(C8) = Uanis(C11) = Uanis(C9) = Uanis(C10) = Uanis(C1)
Uanis(C12) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C14) = Uanis(C13) =
Uanis(C18) = Uanis(C19) = Uanis(C1A) = Uanis(C1D) = Uanis(C1C) = Uanis(C1B)
4. Others
 Fixed Sof: C20(0.5) C1G(0.5) H1G(0.5) C23(0.5) H23(0.5) C25(0.5) H25(0.5)
 C24(0.5) H24(0.5) C1F(0.5) H1F(0.5) C21(0.5) H21(0.5) C1E(0.5) C22(0.5)
 H22(0.5) C1H(0.5) H1H(0.5) C1J(0.5) H1J(0.5) C1I(0.5) H1I(0.5) C0(0.5) C2(0.5)
 H2(0.5) C5(0.5) H5(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C7(0.5) H7(0.5)
 C12(0.5) H12(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5)
 C14(0.5) H14(0.5) C13(0.5) C6(0.5) C8(0.5) H8(0.5) C11(0.5) H11(0.5) C9(0.5)
 H9(0.5) C10(0.5) H10(0.5) C1(0.5) H1(0.5) C18(0.5) H18(0.5) C19(0.5) C1A(0.5)
 H1A(0.5) C1D(0.5) H1D(0.5) C1C(0.5) H1C(0.5) C1B(0.5) H1B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00X(H00X), C00Z(H00Z), C012(H012), C1G(H1G), C23(H23), C25(H25),
 C24(H24), C1F(H1F), C01A(H01A), C01C(H01C), C01H(H01H), C01I(H01I), C01J(H01J),
  C01L(H01L), C01M(H01M), C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S),
 C01U(H01U), C01W(H01W), C01Y(H01Y), C022(H022), C024(H024), C026(H026),
 C027(H027), C02A(H02A), C21(H21), C22(H22), C1H(H1H), C1J(H1J), C1I(H1I),
 C02D(H02D), C02E(H02E), C02F(H02F), C02I(H02I), C02K(H02K), C02M(H02M),
 C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C2(H2), C5(H5), C3(H3), C4(H4),
  C7(H7), C02V(H02V), C02W(H02W), C12(H12), C15(H15), C16(H16), C17(H17),
 C14(H14), C02Y(H02Y), C02Z(H02Z), C031(H031), C033(H033), C036(H036),
 C037(H037), C038(H038), C039(H039), C03A(H03A), C03B(H03B), C03C(H03C),
 C03D(H03D), C03I(H03I), C03K(H03K), C03M(H03M), C03O(H03O), C03Q(H03Q),
 C03T(H03T), C03V(H03V), C03W(H03W), C03Y(H03Y), C03Z(H03Z), C8(H8), C11(H11),
 C9(H9), C10(H10), C1(H1), C18(H18), C1A(H1A), C1D(H1D), C1C(H1C), C1B(H1B)
5.b Fitted hexagon refined as free rotating group:
 C20(C1G,C23,C25,C24,C1F), C21(C1E,C22,C1H,C1J,C1I), C0(C2,C5,C3,C4,C7),
 C12(C15,C16,C17,C14,C13), C6(C8,C11,C9,C10,C1), C18(C19,C1A,C1D,C1C,C1B)
5.c Idealised Me refined as rotating group:
 C03H(H03H,H03J,H03L), C03X(H03E,H03F,H03G)
;
_shelx_res_checksum              60098
_shelx_hkl_checksum              7981
_olex2_submission_special_instructions 'No special instructions were received'