Luminescent iridium(iii) complexes of N-heterocyclic carbene ligands prepared using the 'click reaction'.
Karmis, Rebecca E.; Carrara, Serena; Baxter, Amy A.; Hogan, Conor F.; Hulett, Mark D.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9998–10010; doi:10.1039/c9dt01362h

data_7700130
_publ_section_title
;
 Luminescent iridium(iii) complexes of N-heterocyclic carbene ligands
 prepared using the 'click reaction'.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9998
_journal_page_last               10010
_journal_paper_doi               10.1039/c9dt01362h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'F6 P, C20 H20 N5'
_chemical_formula_sum            'C20 H20 F6 N5 P'
_chemical_formula_weight         475.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.64361(15)
_cell_length_b                   16.6534(4)
_cell_length_c                   26.2220(4)
_cell_measurement_reflns_used    8003
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      77.1710
_cell_measurement_theta_min      3.0980
_cell_volume                     4211.22(14)
_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      172.99(10)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14267
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        65.063
_diffrn_reflns_theta_max         65.063
_diffrn_reflns_theta_min         3.144
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2449 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.505(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         6850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+1.8776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1498
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                6302
_reflns_number_total             6850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01362h2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7700130--7700132.cif.'
_cod_original_cell_volume        4211.22(13)
_cod_database_code               7700130
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C24(H24A,H24B), C7(H7A,H7B), C34(H34A,H34B), C14(H14A,H14B),
 C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C29(H29), C21(H21), C9(H9), C13(H13), C6(H6), C22(H22), C23(H23),
 C20(H20), C16(H16), C11(H11), C40(H40), C31(H31), C26(H26), C10(H10), C32(H32),
  C33(H33), C36(H36), C12(H12), C39(H39), C30(H30), C19(H19), C3(H3), C17(H17),
 C18(H18), C38(H38), C2(H2), C37(H37)
;
_olex2_submission_special_instructions 'No special instructions were received'