Postmodification of the electronic properties by addition of π-stacking additives in N-heterocyclic carbene complexes with extended polyaromatic systems.
Valdés, Hugo; Poyatos, Macarena; Peris, Eduardo; Inorganic chemistry 54 (2015) 3654–3659; doi:10.1021/acs.inorgchem.5b00250

data_4346080
_publ_section_title
;
 Postmodification of the electronic properties by addition of \p-stacking
 additives in N-heterocyclic carbene complexes with extended polyaromatic
 systems.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3654
_journal_page_last               3659
_journal_paper_doi               10.1021/acs.inorgchem.5b00250
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C39 H40 I Ir N4'
_chemical_formula_sum            'C39 H40 I Ir N4'
_chemical_formula_weight         883.90
_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_primary     iterative
_audit_creation_date             2014-03-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                82.045(4)
_cell_angle_beta                 70.514(3)
_cell_angle_gamma                79.321(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7342(3)
_cell_length_b                   11.9737(5)
_cell_length_c                   13.7298(6)
_cell_measurement_reflns_used    18110
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.7960
_cell_measurement_theta_min      3.4830
_cell_volume                     1629.18(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.8459
_diffrn_measurement_details
;
  1 omega  -20.00   29.70   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   90.0000 71

  2 omega -104.00  -55.00   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  178.0000   30.0000 70

  3 omega  -65.00   46.30   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -38.0000  -90.0000 159

  4 omega   34.00  106.10   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814 -178.0000  -90.0000 103

  5 omega   35.00  107.10   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  178.0000   60.0000 103

  6 omega  -20.00   99.00   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   77.0000  -90.0000 170

  7 omega  -65.00   46.30   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -38.0000    0.0000 159

  8 omega  -20.00   29.70   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   30.0000 71

  9 omega -106.00  -57.00   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877 -178.0000  -30.0000 70

 10 omega  -20.00   29.70   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000  120.0000 71

 11 omega  -20.00   59.10   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -99.0000 -120.0000 113

 12 omega  -17.00   94.30   0.7000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   38.0000   60.0000 159
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0174223000
_diffrn_orient_matrix_UB_12      0.0552538000
_diffrn_orient_matrix_UB_13      -0.0045837000
_diffrn_orient_matrix_UB_21      0.0122519000
_diffrn_orient_matrix_UB_22      0.0036333000
_diffrn_orient_matrix_UB_23      -0.0543195000
_diffrn_orient_matrix_UB_31      -0.0676090000
_diffrn_orient_matrix_UB_32      0.0243485000
_diffrn_orient_matrix_UB_33      0.0072156000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34739
_diffrn_reflns_theta_full        29.2138
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.080
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.8017
_exptl_crystal_description       needle
_exptl_crystal_F_000             860.9141
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.1383
_exptl_crystal_size_min          0.0705
_refine_diff_density_max         2.3252
_refine_diff_density_min         -1.0692
_refine_diff_density_rms         0.2223
_refine_ls_d_res_high            0.7281
_refine_ls_d_res_low             7.1066
_refine_ls_goodness_of_fit_ref   1.0562
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     407
_refine_ls_number_reflns         8079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0562
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+2.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7124
_reflns_number_total             8079
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5b00250_si_002.cif
_cod_data_source_block           str1624_complex_5-H
_cod_original_cell_volume        1629.18(12)
_cod_database_code               4346080
_chemical_oxdiff_formula         'C38 H30 N4 I Ir'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C39(H39), C36(H36), C35(H35), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C7(H7a,H7b), C4(H4a,H4b), C8(H8a,H8b), C34(H34a,H34b), C3(H3a,
 H3b), C6(H6a,H6b), C37(H37a,H37b), C38(H38a,H38b), C33(H33a,H33b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C20(H20), C30(H30), C25(H25), C17(H17), C21(H21), C18(H18),
 C26(H26), C16(H16), C24(H24)
2.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C9(H9a,H9b,H9c)
;