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_7707217
_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         'C130 H92 Ir2 N8 O12 S, 7(C2 H3 N)'
_chemical_formula_sum            'C144 H113 Ir2 N15 O12 S'
_chemical_formula_weight         2661.95
_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
_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                105.080(3)
_cell_angle_beta                 101.124(3)
_cell_angle_gamma                90.032(4)
_cell_formula_units_Z            2
_cell_length_a                   14.2021(15)
_cell_length_b                   19.393(2)
_cell_length_c                   23.025(2)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.54
_cell_volume                     5999.5(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  0.0541
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98817
_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         1.870
_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    2.305
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0666 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.8615.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1582
_refine_ls_number_reflns         23568
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0168P)^2^+12.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18831
_reflns_number_total             23568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00820j2.cif
_cod_data_source_block           st36h
_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        5999.5(11)
_cod_database_code               7707217
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.724
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C02U
 1.4 with sigma of 0.01
 C2-C04B
 1.35 with sigma of 0.02
 O0-C1 \\sim O0-C0
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C04T) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S003) = Uanis(S004)
Uanis(C5) = Uanis(C2)
Uanis(O0) = Uanis(C0) = Uanis(C1)
Uanis(S003) = Uanis(C2) = Uanis(C5) = Uanis(S004)
4. Others
 Fixed Sof: S003(0.5) S004(0.5) H04D(0.5) H04E(0.5) H04G(0.5) H04F(0.5)
 C0(0.5) H0A(0.5) H0B(0.5) H0C(0.5) C2(0.5) H2(0.5) C5(0.5) H5(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) H1C(0.5)
 Fixed X: C2(0.14624) C5(0.295469)
 Fixed Y: C2(0.88299) C5(0.91521)
 Fixed Z: C2(0.80014) C5(0.821921)
5.a Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C017(H017), C018(H018), C019(H019), C01A(H01A), C01H(H01H),
 C01J(H01J), C01L(H01L), C01T(H01T), C01V(H01V), C01X(H01X), C022(H022),
 C025(H025), C026(H026), C027(H027), C02A(H02A), C02B(H02B), C02D(H02D),
 C02E(H02E), C02G(H02G), C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N),
 C02O(H02O), C02Q(H02Q), C02R(H02R), C02T(H02T), C02V(H02V), C02W(H02W),
 C02X(H02X), C02Y(H02Y), C02Z(H02Z), C031(H031), C032(H032), C033(H033),
 C035(H035), C037(H037), C03A(H03A), C03B(H03B), C03C(H03C), C03D(H03D),
 C03E(H03E), C03F(H03F), C03G(H03G), C03H(H03H), C03I(H03I), C03J(H03J),
 C03K(H03K), C03M(H03M), C03N(H03N), C03P(H03Q), C03S(H03X), C03V(H03Y),
 C03X(H03Z), C03Z(H03), C040(H040), C041(H041), C043(H043), C044(H044),
 C049(H049), C04A(H04D), C04A(H04E), C04B(H04G), C04B(H04F), C04E(H04K),
 C04K(H04L), C04P(H04P), C04S(H04S), C2(H2), C5(H5)
5.b Idealised Me refined as rotating group:
 C03O(H03L,H03O,H03P), C03Q(H03R,H03S,H03T), C03R(H03U,H03V,H03W), C03W(H3,H,
 HA), C03Y(H1,HB,HC), C045(H04A,H04B,H04C), C048(H04Z,HD,HE), C04D(H04H,H04I,
 H04J), C04G(H04X,H04Y,HF), C04I(H04,HG,HH), C04O(H04U,H04V,H04W), C04Q(H4,HI,
 HJ), C04R(H04M,H04N,H04O), C04T(H04Q,H04R,H04T), C0(H0A,H0B,H0C)
;
_shelx_res_checksum              38584
_shelx_hkl_checksum              94303
_olex2_submission_special_instructions 'No special instructions were received'