A C3v-symmetrical tribenzotriquinacene-based threefold N-heterocyclic carbene. Coordination to rhodium(I) and stereoelectronic properties
Candela Segarra; Jens Linke; Elena Mas-Marza; Dietmar Kuck; Eduardo Peris; Chem.Commun. 49 (2013) 10572–; doi:10.1039/c3cc46155f

data_7110006
_publ_section_title
;
 A C3v-symmetrical tribenzotriquinacene-based threefold N-heterocyclic
 carbene. Coordination to rhodium(I) and stereoelectronic properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              10572
_journal_paper_doi               10.1039/c3cc46155f
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C53 H72 N6, 3(B F4)'
_chemical_formula_sum            'C53 H72 B3 F12 N6'
_chemical_formula_weight         1053.60
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           185
_space_group_name_Hall           'P 6c -2'
_space_group_name_H-M_alt        'P 63 c m'
_symmetry_space_group_name_Hall  'P 6c -2'
_symmetry_space_group_name_H-M   'P 63 c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-10
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Apr  9 2013 14:10:59, GUI svn.r4452)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.7431(5)
_cell_length_b                   15.7431(5)
_cell_length_c                   12.5624(5)
_cell_measurement_reflns_used    4800
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      69.0500
_cell_measurement_theta_min      5.5960
_cell_volume                     2696.40(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_details
;
  1 omega -117.00  -10.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -37.0000  -30.0000 107

  2 omega  -45.00  -11.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   30.0000    0.0000 34

  3 omega   53.00   90.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -30.0000  -90.0000 37

  4 omega   29.00   87.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -30.0000   60.0000 58

  5 omega  103.00  172.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  111.0000  150.0000 69

  6 omega   46.00   96.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -45.0000    0.0000 50

  7 omega   27.00   92.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000    0.0000 65

  8 omega -116.00   -5.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000 -180.0000 111

  9 omega   30.00  103.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057 -136.0000 -145.0000 73

 10 omega -147.00  -37.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -45.0000  -90.0000 110

 11 omega   30.00   98.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -45.0000  150.0000 68

 12 omega   70.00  178.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   30.0000 -180.0000 108

 13 omega   27.00  115.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000 -180.0000 88

 14 omega   27.00  178.00   1.0000   21.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   15.0000   90.0000 151
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0844165000
_diffrn_orient_matrix_UB_12      -0.0952818000
_diffrn_orient_matrix_UB_13      -0.0472018000
_diffrn_orient_matrix_UB_21      -0.0349600000
_diffrn_orient_matrix_UB_22      -0.0399260000
_diffrn_orient_matrix_UB_23      0.1132595000
_diffrn_orient_matrix_UB_31      -0.0664392000
_diffrn_orient_matrix_UB_32      0.0458262000
_diffrn_orient_matrix_UB_33      0.0004159000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16021
_diffrn_reflns_theta_full        72.47
_diffrn_reflns_theta_max         72.47
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whitish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1899
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1620P)^2^+0.4171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                1704
_reflns_number_total             1899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46155f.txt
_cod_data_source_block           str1478
_cod_original_cell_volume        2696.41(16)
_cod_database_code               7110006
_chemical_oxdiff_formula         'C53 H75 N6 B3 F12'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C13(H13)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C5(H5A,H5B,H5C)
;