25,26,27,28-Tetrapropoxycalix[4]arene-5,17-dicarbonitrile
Budka, Jan; Eigner, Václav; Holakovský, Roman; Kovaříček, Petr; Loužilová, Tereza; Acta Crystallographica Section E 66 (2010) o419–o420; doi:10.1107/S1600536810002242

data_2225075
_publ_section_title
;
 25,26,27,28-Tetrapropoxycalix[4]arene-5,17-dicarbonitrile
;
_journal_coeditor_code           OM2307
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o419
_journal_page_last               o420
_journal_paper_doi               10.1107/S1600536810002242
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C42 H46 N2 O4'
_chemical_formula_moiety         'C42 H46 N2 O4'
_chemical_formula_sum            'C42 H46 N2 O4'
_chemical_formula_weight         642.84
_chemical_name_systematic
;
25,26,27,28-Tetrapropoxycalix[4]arene-5,17-dicarbonitrile
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.987(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.398(4)
_cell_length_b                   10.6491(12)
_cell_length_c                   34.391(2)
_cell_measurement_reflns_used    3818
_cell_measurement_temperature    150
_cell_measurement_theta_max      78
_cell_measurement_theta_min      4
_cell_volume                     7087.0(17)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.1917
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            44656
_diffrn_reflns_theta_full        69.433
_diffrn_reflns_theta_max         78.014
_diffrn_reflns_theta_min         4.347
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         7906
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.0244808
_refine_ls_shift/su_mean         7.8232179
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 20.7 2.42 17.0 5.57
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0893
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                7906
_reflns_number_total             14658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2307.cif
_cod_data_source_block           I
_cod_original_cell_volume        7086.9(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225075
_cod_database_fobs_code          2225075