Multinuclear Alkali Metal Complexes of a Triphenylene-Based Hexamine and the Transmetalation to Tris(N-heterocyclic tetrylenes) (Ge, Sn, Pb).
Zhong, Fei; Yang, Xiaodong; Shen, Lingyi; Zhao, Yanxia; Ma, Hongwei; Wu, Biao; Yang, Xiao-Juan; Inorganic chemistry 55 (2016) 9112–9120; doi:10.1021/acs.inorgchem.6b01743

data_4348861
_publ_section_title
;
 Multinuclear Alkali Metal Complexes of a Triphenylene-Based Hexamine and
 the Transmetalation to Tris(N-heterocyclic tetrylenes) (Ge, Sn, Pb).
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9112
_journal_page_last               9120
_journal_paper_doi               10.1021/acs.inorgchem.6b01743
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'2(C98 H129 N6 Na O4), 2(C98 H132 N6 Na O4), 3(C6), 2(C12 H27 Na O6), 2(C4 H10 O2), 2(C10.5 Na O6.2)'
_chemical_formula_sum            'C466 H710 N24 Na8 O44'
_chemical_formula_weight         7536.46
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                89.694(4)
_cell_angle_beta                 88.260(4)
_cell_angle_gamma                70.273(4)
_cell_formula_units_Z            1
_cell_length_a                   18.473(5)
_cell_length_b                   23.229(6)
_cell_length_c                   28.377(7)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.81
_cell_measurement_theta_min      2.34
_cell_volume                     11457(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
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_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.2408
_diffrn_reflns_Laue_measured_fraction_full 0.957
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_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.957
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_diffrn_reflns_theta_max         24.652
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_diffrn_source_current           30.0
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
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_exptl_crystal_density_meas      1.095
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
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_exptl_transmission_factor_min   0.4380
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         37157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.2488
_refine_ls_R_factor_gt           0.1047
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+26.3974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13781
_reflns_number_total             37157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01743_si_002.cif
_cod_data_source_block           1
_cod_database_code               4348861
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.978
_shelx_hkl_checksum              9331
_shelx_res_checksum              35749
_shelx_shelxl_version_number     2014/7