Crystal structure of a four-layered [3.3](3,5)pyridinophane
Shibahara, Masahiko; Watanabe, Motonori; Matsumoto, Taisuke; Goto, Kenta; Shinmyozu, Teruo; Acta Crystallographica Section E 70 (2014) 447–450; doi:10.1107/S1600536814023691

data_2240145
_publ_section_title
;
 Crystal structure of a four-layered [3.3](3,5)pyridinophane
;
_journal_coeditor_code           HB7300
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              447
_journal_page_last               450
_journal_paper_doi               10.1107/S1600536814023691
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C40 H46 N2'
_chemical_formula_moiety         'C40 H46 N2'
_chemical_formula_sum            'C40 H46 N2'
_chemical_formula_weight         554.79
_chemical_name_common            four-layered[3.3](3,5)pyridinophane
_chemical_name_systematic
12,30-Diazaheptacyclo[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
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                75.619(16)
_cell_angle_beta                 88.369(17)
_cell_angle_gamma                86.755(17)
_cell_formula_units_Z            2
_cell_length_a                   6.1377(15)
_cell_length_b                   14.643(4)
_cell_length_c                   17.519(4)
_cell_measurement_reflns_used    20167
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.242
_cell_measurement_theta_min      3.120
_cell_volume                     1522.6(7)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
<i>Yadokari-XG 2009</i> (Wakita, 2001; Kabuto <i>et al.</i>,
2009)
;
_computing_publication_material
;
<i>Yadokari-XG 2009</i> (Wakita, 2001; Kabuto <i>et al.</i>,
2009),
ORTEP-3 for Windows (Farrugia, 2012),
Mercury (Macrae <i>et al.</i>,  2006),
publCIF (Westrip, 2010) and enCIFer (Allen <i>et al.</i>,
2004)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR2011 (Camalli <i>et al.</i>,  2012)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20167
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.120
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0985P)^2^+0.5512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2044
_reflns_number_gt                4455
_reflns_number_total             5396
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7300sup1.cif
_cod_data_source_block           I
_cod_database_code               2240145
_cod_database_fobs_code          2240145
_shelx_hkl_checksum              41181
_shelx_res_checksum              34774
_shelxl_version_number           2.014