Iridium(iii) N-heterocyclic carbene complexes: an experimental and theoretical study of structural, spectroscopic, electrochemical and electrogenerated chemiluminescence properties.
Barbante, Gregory J.; Doeven, Egan H.; Francis, Paul S.; Stringer, Bradley D.; Hogan, Conor F.; Kheradmand, Peyman R.; Wilson, David J. D.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 8564–8576; doi:10.1039/c4dt03378g

data_7033917
_publ_section_title
;
 Iridium(iii) N-heterocyclic carbene complexes: an experimental and
 theoretical study of structural, spectroscopic, electrochemical and
 electrogenerated chemiluminescence properties.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8564
_journal_page_last               8576
_journal_paper_doi               10.1039/c4dt03378g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C41 H31 Ir N5, F6 P'
_chemical_formula_sum            'C41 H31 F6 Ir N5 P'
_chemical_formula_weight         930.88
_chemical_name_systematic        4.PF6
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-30 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3280(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.14380(14)
_cell_length_b                   15.66023(14)
_cell_length_c                   19.33573(19)
_cell_measurement_temperature    173.2
_cell_volume                     3605.53(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61518
_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         26.021
_diffrn_reflns_theta_min         2.469
_exptl_absorpt_coefficient_mu    3.817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.74911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+3.6043P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6508
_reflns_number_total             7102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03378g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7033915--7033917.cif.'
_cod_original_cell_volume        3605.53(7)
_cod_database_code               7033917
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C15A-C16A = C16A-C17A = C17A-C18A = C18A-C19A = C19A-C14 = C14-C15A
 1.39 with sigma of 0.001
 C15-C16 = C16-C17 = C17-C18 = C18-C19 = C19-C14 = C14-C15
 1.39 with sigma of 0.001
3. Restrained planarity
 C15A, C16A, C17A, C18A, C19A, C14
 with sigma of 0.1
 C15, C16, C17, C18, C19, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C19) = Uanis(C19A)
Uanis(C18) = Uanis(C18A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
Uanis(C17) = Uanis(C17A)
5. Others
 Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=
 Sof(H15A)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(C19)=Sof(H19)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=FVAR(1)
;
_shelx_res_checksum              6066
_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'