Open-shell doublet character in a hexaazatrinaphthylene trianion complex
Jani O. Moilanen; Benjamin M. Day; Thomas Pugh; Richard A. Layfield; Chem.Commun. 51 (2015) 11478–; doi:10.1039/C5cc04004C

data_7117422
_publ_section_title
;
 Open-shell doublet character in a hexaazatrinaphthylene trianion complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              11478
_journal_paper_doi               10.1039/C5cc04004C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C111 H135 Mg3 N12, 1(C7 H8)'
_chemical_formula_sum            'C118 H143 Mg3 N12'
_chemical_formula_weight         1802.37
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-05 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.9267(3)
_cell_length_b                   15.9267(3)
_cell_length_c                   24.0860(9)
_cell_measurement_reflns_used    11457
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      27.9950
_cell_measurement_theta_min      3.8810
_cell_volume                     5291.1(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -54.00   76.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       19.4509    0.0000  -90.0000 130

  2 omega  -11.00   90.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       19.4509   77.0000   60.0000 101

  3 omega  -29.00    7.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571  -77.0000  150.0000 36

  4 omega   60.00   96.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       19.4509 -178.0000   60.0000 36

  5 omega  -48.00   51.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571   77.0000  -90.0000 99

  6 omega  -95.00  -60.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571  178.0000   30.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0246075000
_diffrn_orient_matrix_UB_12      -0.0212314000
_diffrn_orient_matrix_UB_13      -0.0251804000
_diffrn_orient_matrix_UB_21      -0.0447812000
_diffrn_orient_matrix_UB_22      -0.0231403000
_diffrn_orient_matrix_UB_23      0.0144631000
_diffrn_orient_matrix_UB_31      -0.0058359000
_diffrn_orient_matrix_UB_32      0.0407037000
_diffrn_orient_matrix_UB_33      -0.0048953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44033
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1942
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3690
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0551P)^2^+4.1070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                3040
_reflns_number_total             3690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04004c2.cif
_cod_data_source_block           Mg3HAN
_cod_original_cell_volume        5291.1(3)
_cod_database_code               7117422
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C183H135N12Mg3
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C30-C24
 1.52 with sigma of 0.02
 C29-C30 = C30-C25
 2.5 with sigma of 0.02
3. Others
 Fixed Sof: C24(0.16667) C29(0.16667) H29(0.16667) C28(0.16667) H28(0.16667)
 C27(0.16667) H27(0.16667) C26(0.16667) H26(0.16667) C25(0.16667) H25(0.16667)
 C30(0.16667) H30A(0.16667) H30B(0.16667) H30C(0.16667)
4.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C14(H14), C15(H15), C16(H16),
 C29(H29), C28(H28), C27(H27), C26(H26), C25(H25)
4.c Fitted hexagon refined as free rotating group:
 C24(C29,C28,C27,C26,C25)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              14922
_shelx_hkl_checksum              30717
_olex2_submission_special_instructions 'No special instructions were received'