Four-layered [3.3]metacyclophane with ethenetetracarbonitrile
Shibahara, Masahiko; Watanabe, Motonori; Goto, Kenta; Shinmyozu, Teruo; Acta Crystallographica Section E 70 (2014) o625–o626; doi:10.1107/S1600536814009362

data_2239511
_publ_section_title
;
 Four-layered [3.3]metacyclophane with ethenetetracarbonitrile
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o625
_journal_page_last               o626
_journal_paper_doi               10.1107/S1600536814009362
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C42 H48, 2C6 N4'
_chemical_formula_moiety         'C54 H48 N8'
_chemical_formula_sum            'C54 H48 N8'
_chemical_formula_weight         809.03
_chemical_name_systematic
'Heptacyclo[21.13.1.1^5,19^.1^6,18^.1^10,14^.1^24,36^.1^28,32^]dotetraconta-1(37),5(40),6(41),10(42),11,13,18,23,28,30,32(39),36(38)-dodecaene--ethenetetracarbonitrile (1/2)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.365(14)
_cell_angle_beta                 99.134(13)
_cell_angle_gamma                107.683(13)
_cell_formula_units_Z            1
_cell_length_a                   9.563(3)
_cell_length_b                   10.101(4)
_cell_length_c                   11.679(4)
_cell_measurement_reflns_used    13845
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     1045.9(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'CrystalStructure (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXD</i> (Schneider & Sheldrick, 2002)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17470
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4775
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1296P)^2^+0.1947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1782
_reflns_number_gt                4141
_reflns_number_total             4775
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            gw2145sup1.cf
_cod_data_source_block           I
_cod_database_code               2239511
_cod_database_fobs_code          2239511