Cationic iridium complexes with an alkyl-linked bulky group at the cyclometalating ligand: synthesis, characterization, and suppression of phosphorescence concentration-quenching
Song, Yongjun; Ren, Hao; Meng, Xianwen; He, Lei; New Journal of Chemistry 45 (2021) 15312–15320; doi:10.1039/D1NJ02375F

data_7060807
_publ_section_title
;
 Cationic iridium complexes with an alkyl-linked bulky group at the
 cyclometalating ligand: synthesis, characterization, and suppression of
 phosphorescence concentration-quenching
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15312
_journal_page_last               15320
_journal_paper_doi               10.1039/D1NJ02375F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C64 H51 Ir N5, F6 P, C H Cl3'
_chemical_formula_sum            'C65 H52 Cl3 F6 Ir N5 P'
_chemical_formula_weight         1346.64
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                70.82(3)
_cell_angle_beta                 79.66(3)
_cell_angle_gamma                74.70(3)
_cell_formula_units_Z            2
_cell_length_a                   12.775(3)
_cell_length_b                   15.234(3)
_cell_length_c                   16.485(3)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.4510
_cell_volume                     2907.5(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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
;
????
;
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.8689
	          2theta: -20.2028
scan:
	Number of images: 340
	           Slice: -110.0000 - 60.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 44.8689
	          2theta: -20.2028
scan:
	Number of images: 120
	           Slice: -110.0000 - -50.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.8689
	          2theta: -20.2028
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0307
_diffrn_orient_matrix_UB_12      -0.0551
_diffrn_orient_matrix_UB_13      -0.0518
_diffrn_orient_matrix_UB_21      0.0681
_diffrn_orient_matrix_UB_22      0.0047
_diffrn_orient_matrix_UB_23      -0.0206
_diffrn_orient_matrix_UB_31      -0.0017
_diffrn_orient_matrix_UB_32      -0.0382
_diffrn_orient_matrix_UB_33      0.0520
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27236
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.527
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.609
_refine_diff_density_min         -2.274
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         13141
_refine_ls_number_restraints     1002
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+11.4496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1850
_reflns_number_gt                12116
_reflns_number_total             13141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj02375f2.cif
_cod_data_source_block           bww16096
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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 7060807.cif.
;
_cod_original_cell_volume        2907.5(10)
_cod_database_code               7060807
_diffrn_number_total             13149
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C43(H43), C119(H119), C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C65(H65A,H65B)
3.c Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C16(H16), C17(H17), C32(H32), C39(H39), C44(H44), C46(H46),
 C51(H51), C53(H53), C56(H56), C70(H70), C72(H72), C73(H73), C76(H76), C80(H80),
  C83(H83), C85(H85), C88(H88), C89(H89), C90(H90), C92(H92), C94(H94),
 C103(H103), C105(H105), C112(H112), C114(H114), C117(H117), C118(H118),
 C120(H120), C125(H125), C128(H128), C130(H130), C131(H131), C133(H133),
 C137(H137), C140(H140), C142(H142), C146(H146), C148(H148), C149(H149),
 C151(H151), C153(H153), C164(H164), C170(H170), C0AA(H0AA)
;
_olex2_submission_special_instructions 'No special instructions were received'