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_7707218
_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 F4 Ir2 N8 O4 S, 4.5(C2 H3 N)'
_chemical_formula_sum            'C131 H85.5 F4 Ir2 N12.5 O4 S'
_chemical_formula_weight         2391.07
_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                104.068(4)
_cell_angle_beta                 107.253(4)
_cell_angle_gamma                93.552(4)
_cell_formula_units_Z            2
_cell_length_a                   17.471(2)
_cell_length_b                   17.750(2)
_cell_length_c                   18.145(2)
_cell_measurement_reflns_used    9048
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.36
_cell_volume                     5157.7(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84068
_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         26.000
_diffrn_reflns_theta_min         1.930
_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    2.671
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0899 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.8514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             2394
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.963
_refine_diff_density_min         -1.802
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         20266
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+16.3796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17023
_reflns_number_total             20266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00820j2.cif
_cod_data_source_block           st39h
_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_cell_volume        5157.9(10)
_cod_original_formula_sum        'C131 H85.50 F4 Ir2 N12.50 O4 S'
_cod_database_code               7707218
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.740
_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
 N1-C2
 1.15 with sigma of 0.01
 C1-N2
 1.15 with sigma of 0.01
 C3-C2 \\sim C5-C1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C042 \\sim C041: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Uanis(C049) \\sim Ueq, Uanis(C04A) \\sim Ueq, Uanis(N04B) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(N1) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(C1) = Uanis(C5)
4. Others
 Fixed Sof: C049(0.5) C04A(0.5) H04G(0.5) H04H(0.5) H04I(0.5) N04B(0.5)
 N1(0.5) C2(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) N2(0.5) C1(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) H5C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C010(H010), C011(H011), C015(H015), C017(H017), C019(H019),
 C01D(H01D), C01E(H01E), C01H(H01H), C01J(H01J), C01M(H01M), C01S(H01S),
 C01T(H01T), C01U(H01U), C01X(H01X), C01Z(H01Z), C020(H020), C022(H022),
 C025(H025), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02E(H02E),
 C02F(H02F), C02H(H02H), C02J(H02J), C02L(H02L), C02M(H02M), C02N(H02N),
 C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T), C02U(H02U),
 C02V(H02V), C02W(H02W), C02Y(H02Y), C02Z(H02Z), C030(H030), C031(H031),
 C032(H032), C033(H033), C034(H034), C035(H035), C037(H037), C038(H038),
 C03A(H03A), C03B(H03B), C03C(H03C), C03D(H03D), C03E(H03E), C03F(H03F),
 C03G(H03G), C03H(H03H), C03I(H03I), C03J(H03J), C03K(H03K), C03L(H03L),
 C03M(H03M), C03N(H03N), C03O(H03O), C03P(H03P), C03Q(H03Q), C03R(H03R),
 C03T(H03T), C03U(H03U), C03W(H03W), C03X(H03X), C041(H041), C042(H042)
5.b Idealised Me refined as rotating group:
 C03V(H03S,H03V,H03Y), C043(H04A,H04B,H04C), C044(H04D,H04E,H04F), C04A(H04G,
 H04H,H04I), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              68031
_shelx_hkl_checksum              37074
_olex2_submission_special_instructions 'No special instructions were received'