<i>C</i>-Methylcalix[4]resorcinarene–1,4-bis(pyridin-3-yl)-2,3-diaza-1,3-butadiene (1/2)
Udachin, Konstantin A.; Zaman, Md. Badruz; Ripmeester, John A.; Acta Crystallographica Section E 68 (2012) o261–o262; doi:10.1107/S1600536811054717

data_2233651
_publ_section_title
;
 <i>C</i>-Methylcalix[4]resorcinarene--1,4-bis(pyridin-3-yl)-2,3-diaza-1,3-butadiene
 (1/2)
;
_journal_coeditor_code           VM2143
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o261
_journal_page_last               o262
_journal_paper_doi               10.1107/S1600536811054717
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '2C12 H10 N4, C32 H32 O8'
_chemical_formula_moiety         '2(C12 H10 N4), C32 H32 O8'
_chemical_formula_sum            'C56 H52 N8 O8'
_chemical_formula_weight         965.06
_chemical_name_common
;
<i>C</i>-Methylcalix[4]resorcinarene--1,4-bis(pyridin-3-yl)-2,3-diaza-
1,3-butadiene (1/2)
;
_chemical_name_systematic
;
2,9,15,22-tetramethylpentacyclo[21.3.1.1^10,14^.0^3,8^.0^16,21^]octacosa-
1(27),3(8),4,6,10(28),11,13,16,18,20,23,25-dodecaen-
5,6,11,13,18,19,24,26-octol--1,4-bis(pyridin-3-yl)-2,3-diaza-1,3-butadiene (1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.324(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2998(10)
_cell_length_b                   26.232(2)
_cell_length_c                   16.1097(13)
_cell_measurement_reflns_used    280
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     4904.9(7)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'ATOMS (Dowty, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58266
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         12755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0601P)^2^+0.3967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                7952
_reflns_number_total             12755
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            vm2143.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233651
_cod_database_fobs_code          2233651