Tuning the electrochemiluminescent properties of iridium complexes of N-heterocyclic carbene ligands.
Quan, Linh M.; Stringer, Bradley D.; Haghighatbin, Mohammad A.; Agugiaro, Johnny; Barbante, Gregory J.; Wilson, David J. D.; Hogan, Conor F.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 653–663; doi:10.1039/c8dt04433c

data_7048309
_publ_section_title
;
 Tuning the electrochemiluminescent properties of iridium complexes of
 N-heterocyclic carbene ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              653
_journal_page_last               663
_journal_paper_doi               10.1039/c8dt04433c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H26 Cl F4 Ir N4, C2 H3 N'
_chemical_formula_sum            'C36 H29 Cl F4 Ir N5'
_chemical_formula_weight         835.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-23 deposited with the CCDC.
2018-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.264(3)
_cell_angle_beta                 105.973(3)
_cell_angle_gamma                98.494(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0031(3)
_cell_length_b                   12.7459(4)
_cell_length_c                   15.4060(5)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.3129
_cell_measurement_theta_min      2.8793
_cell_volume                     1602.56(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14873
_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         26.369
_diffrn_reflns_theta_min         2.885
_exptl_absorpt_coefficient_mu    4.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.3275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6065
_reflns_number_total             6542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04433c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7048306--7048309.cif.'
_cod_original_cell_volume        1602.56(9)
_cod_database_code               7048309
_shelx_shelxl_version_number     2014/7
_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.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C5(H5), C9(H9), C15(H15), C8(H8), C18(H18), C19(H19), C21(H21),
 C31(H31), C20(H20), C13(H13), C30(H30), C24(H24), C6(H6), C3(H3), C32(H32),
 C29(H29)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C)
;
_shelx_res_checksum              37893
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with Paratone oil on a glass slide. Suitable single crystals were mounted in Paratone oil on a glass fibre and cooled rapidly to 173 K in a stream of cold N2 using an Oxford low temperature device. '
_olex2_submission_special_instructions 'No special instructions were received'