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_7033916
_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         'C35 H27 Ir N5, F6 P, C H3 O'
_chemical_formula_sum            'C36 H30 F6 Ir N5 O P'
_chemical_formula_weight         885.82
_chemical_name_systematic        3.PF6
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 101.65(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.818(3)
_cell_length_b                   13.881(3)
_cell_length_c                   17.586(4)
_cell_measurement_temperature    173.2
_cell_volume                     3303.6(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.928
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.163
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.86443
_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 yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.910
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0244P)^2^+13.3026P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5849
_reflns_number_total             6505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03378g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7033915--7033917.cif.'
_cod_original_cell_volume        3303.5(12)
_cod_database_code               7033916
_shelxl_version_number           2013-2
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O2)
3. Others
 Sof(H1AD)=Sof(H1AE)=Sof(H1AF)=Sof(O2)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(O1)=FVAR(1)
4.a Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1A(H1AD,H1AE,H1AF)
4.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C17(H17), C3(H3), C23(H23), C4(H4), C32(H32), C33(H33), C24(H24),
 C35(H35), C5(H5), C34(H34), C27(H27), C11(H11), C16(H16), C18(H18), C21(H21),
 C19(H19), C28(H28), C2(H2), C29(H29), C8(H8), C22(H22), C10(H10), C9(H9)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              79748
_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'