Dual phosphorescent emissions from conformers of iridium complex rotors.
Hsu, Yu-Ting; Bhagani, Chandni; Aguilar, Juan A.; Fox, Mark A.; Yufit, Dmitry; Davidson, Ross J.; Beeby, Andrew; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17518–17524; doi:10.1039/d4dt02321h

data_7717207
_publ_section_title
;
 Dual phosphorescent emissions from conformers of iridium complex rotors.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17518
_journal_page_last               17524
_journal_paper_doi               10.1039/d4dt02321h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H41 Cl Ir N3 Si'
_chemical_formula_sum            'C38 H41 Cl Ir N3 Si'
_chemical_formula_weight         795.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2022-01-21 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.7440(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3230(2)
_cell_length_b                   22.6945(4)
_cell_length_c                   11.3723(3)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.59
_cell_measurement_theta_min      2.24
_cell_volume                     3574.88(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  D8Venture
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58858
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.873
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.7335.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         10427
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+3.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                8156
_reflns_number_total             10427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt02321h2.cif
_cod_data_source_block           1_14srv281
_cod_depositor_comments          'Adding full bibliography for 7717207.cif.'
_cod_original_cell_volume        3574.88(12)
_cod_database_code               7717207
_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
 C55B-C54B \\sim C56B-C54B \\sim C56A-C54A \\sim C55A-C54A \\sim C53B-C51B
\\sim C53A-C51A \\sim C52A-
 C51A \\sim C52B-C51B
 with sigma of 0.005
3. Others
 Fixed Sof: C51A(0.5) H51A(0.5) C51B(0.5) H51B(0.5) C52A(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C52B(0.5) H52D(0.5) H52E(0.5) H52F(0.5) C53A(0.5)
 H53A(0.5) H53B(0.5) H53C(0.5) C53B(0.5) H53D(0.5) H53E(0.5) H53F(0.5)
 C54A(0.5) H54A(0.5) C54B(0.5) H54B(0.5) C55A(0.5) H55A(0.5) H55B(0.5)
 H55C(0.5) C55B(0.5) H55D(0.5) H55E(0.5) H55F(0.5) C56A(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C56B(0.5) H56D(0.5) H56E(0.5) H56F(0.5)
4.a Ternary CH refined with riding coordinates:
 C48(H48), C51A(H51A), C51B(H51B), C54A(H54A), C54B(H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21),
 C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31), C41(H41),
  C42(H42), C44(H44), C45(H45)
4.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52A(H52A,H52B,H52C), C52B(H52D,
 H52E,H52F), C53A(H53A,H53B,H53C), C53B(H53D,H53E,H53F), C55A(H55A,H55B,H55C),
 C55B(H55D,H55E,H55F), C56A(H56A,H56B,H56C), C56B(H56D,H56E,H56F)
;
_olex2_submission_special_instructions 'No special instructions were received'