A bis-calixarene from olefin metathesis
Hailu, Shimelis T.; Butcher, Ray J.; Hudrlik, Paul F.; Hudrlik, Anne M.; Acta Crystallographica Section E 68 (2012) o1833–o1834; doi:10.1107/S1600536812022325

data_2235062
_publ_section_title
;
 A bis-calixarene from olefin metathesis
;
_journal_coeditor_code           HG5194
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1833
_journal_page_last               o1834
_journal_paper_doi               10.1107/S1600536812022325
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C74 H68 O8'
_chemical_formula_moiety         'C74 H68 O8'
_chemical_formula_sum            'C74 H68 O8'
_chemical_formula_weight         1085.28
_chemical_name_systematic
;
(15<i>E</i>,40<i>E</i>,60<i>E</i>)-65,74-bis(prop-2-en-1-yloxy)-
13,18,38,43,58,63-hexaoxadodecacyclo[28.26.8.7^20,36^.1^11,45^.1^51,55^.
0^5,57^.0^7,12^.0^19,24^.0^26,64^.0^32,37^.0^44,49^.1^68,72^]tetraheptaconta-
1,3,5(57),7,9,11,15,19(24),20,22,26,28,30(64),32,34,36,40,44(49),45,47,51,53,
55(65),60,68,70,72(74)-heptacosaene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.992(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.075(3)
_cell_length_b                   12.1376(11)
_cell_length_c                   16.9475(7)
_cell_measurement_reflns_used    3491
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      73.6760
_cell_measurement_theta_min      4.6617
_cell_volume                     5958.1(9)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10606
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         73.84
_diffrn_reflns_theta_min         4.67
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.261
_refine_ls_extinction_coef       0.00041(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1069P)^2^+5.7734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2610
_reflns_number_gt                3637
_reflns_number_total             5644
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg5194.cif
_cod_data_source_block           I
_cod_original_cell_volume        5958.1(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235062
_cod_database_fobs_code          2235062