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_7707216
_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(C126 H84 Ir2 N8 O8 S), 2.5(C2 H3 N)'
_chemical_formula_sum            'C68 H49.5 Ir N6.5 O4 S0.5'
_chemical_formula_weight         1229.87
_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                89.263(2)
_cell_angle_beta                 69.208(2)
_cell_angle_gamma                68.446(2)
_cell_formula_units_Z            4
_cell_length_a                   15.9214(10)
_cell_length_b                   19.4903(12)
_cell_length_c                   20.8240(13)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.22
_cell_volume                     5567.1(6)
_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    'XT  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0841
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_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            89775
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.074
_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    2.474
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1215 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.6651.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1406
_refine_ls_number_reflns         21855
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0378P)^2^+21.4798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17339
_reflns_number_total             21855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00820j2.cif
_cod_data_source_block           st38h_1
_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        'C68 H49.50 Ir N6.50 O4 S0.50'
_cod_database_code               7707216
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.723
_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
 C9-C1
 1.5 with sigma of 0.02
 N8-C9
 1.15 with sigma of 0.02
 N00F-C0 \\sim N00F-C6
 with sigma of 0.01
 C17-C02R \\sim C1B-C02R
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C0) = Uanis(C2) = Uanis(C15) = Uanis(C3) = Uanis(C4) = Uanis(C28) =
Uanis(C5) = Uanis(C13) = Uanis(C14) = Uanis(C11) = Uanis(C6) = Uanis(C12)
Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) =
Uanis(C1A) = Uanis(C1B) = Uanis(C1C) = Uanis(C1D) = Uanis(C1E) = Uanis(C1F)
Uanis(C1G) = Uanis(C1I) = Uanis(C1K) = Uanis(C1L) = Uanis(C1J) = Uanis(C1H)
Uanis(N8) = Uanis(C9) = Uanis(C1)
4. Others
 Fixed Sof: C16(0.5) C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5)
 C1C(0.5) H1C(0.5) C1B(0.5) C0(0.5) C2(0.5) H2(0.5) C15(0.5) H15(0.5) C3(0.5)
 H3(0.5) C4(0.5) H4(0.5) C28(0.5) H28(0.5) C22(0.66667) C24(0.66667)
 H24(0.66667) C26(0.66667) H26(0.66667) C27(0.66667) H27(0.66667) C25(0.66667)
 H25(0.66667) C23(0.66667) H23(0.66667) C17(0.5) C18(0.5) H18(0.5) C19(0.5)
 H19(0.5) C20(0.5) H20(0.5) C5(0.5) H5(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
 C11(0.5) H11(0.5) C6(0.5) C12(0.5) H12(0.5) C21(0.5) H21(0.5) N5(0.5) C7(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C1A(0.5) C1G(0.33333) C1I(0.33333)
 H1I(0.33333) C1K(0.33333) H1K(0.33333) C1L(0.33333) H1L(0.33333) C1J(0.33333)
 H1J(0.33333) C1H(0.33333) H1H(0.33333) C1(0.5) H1A(0.5) H1B(0.5) H1G(0.5)
 C9(0.5) N8(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00Z(H00Z), C012(H012), C013(H013), C017(H017), C019(H019),
 C01A(H01A), C01B(H01B), C01F(H01F), C01H(H01H), C01I(H01I), C01L(H01L),
 C01O(H01O), C01P(H01P), C01R(H01R), C01S(H01S), C01U(H01U), C01V(H01V),
 C01W(H01W), C01X(H01X), C024(H024), C025(H025), C1D(H1D), C1E(H1E), C1F(H1F),
 C1C(H1C), C028(H028), C029(H029), C02A(H02D), C02B(H02E), C02D(H02F),
 C02H(H02H), C02I(H02I), C2(H2), C15(H15), C3(H3), C4(H4), C28(H28), C02L(H02L),
  C02M(H02M), C02N(H02N), C02O(H02O), C24(H24), C26(H26), C27(H27), C25(H25),
 C23(H23), C02S(H02S), C02T(H02T), C02V(H02V), C02W(H02W), C02Y(H02Y),
 C02Z(H02Z), C030(H030), C031(H031), C032(H032), C035(H035), C036(H036),
 C038(H038), C039(H039), C03D(H03D), C03F(H03F), C03G(H03G), C03H(H03H),
 C03J(H03J), C03K(H03K), C03L(H03L), C03N(H03N), C03O(H03O), C03P(H03P),
 C18(H18), C03U(H03U), C03X(H03X), C19(H19), C20(H20), C5(H5), C13(H13),
 C14(H14), C11(H11), C12(H12), C21(H21), C1I(H1I), C1K(H1K), C1L(H1L), C1J(H1J),
  C1H(H1H)
5.b Fitted hexagon refined as free rotating group:
 C16(C1D,C1E,C1F,C1C,C1B), C0(C2,C15,C3,C4,C28), C22(C24,C26,C27,C25,C23),
 C5(C13,C14,C11,C6,C12), C1G(C1I,C1K,C1L,C1J,C1H)
5.c Idealised Me refined as rotating group:
 C023(H02A,H02B,H02C), C03I(H03A,H03B,H03C), C03M(H03Q,H03R,H03S), C03R(H03E,
 H03I,H03M), C03W(H03T,H03V,H03W), C047(H04A,H04B,H04C), C049(H04G,H04H,H04I),
 C04A(H04D,H04E,H04F), C10(H10A,H10B,H10C), C1(H1A,H1B,H1G)
;
_shelx_res_checksum              63555
_shelx_hkl_checksum              79083
_olex2_submission_special_instructions 'No special instructions were received'