5,11,17,23,29-Penta-<i>tert</i>-butyl-31,32,33,34,35-pentapropoxycalix[5]arene dichloromethane hemisolvate
Pojarová, Michaela; Dušek, Michal; Budka, Jan; Císařová, Ivana; Makrlík, Emanuel; Acta Crystallographica Section E 67 (2011) o296–o297; doi:10.1107/S1600536811000456

data_2229223
_publ_section_title
;
 5,11,17,23,29-Penta-<i>tert</i>-butyl-31,32,33,34,35-pentapropoxycalix[5]arene
 dichloromethane hemisolvate
;
_journal_coeditor_code           SJ5077
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o296
_journal_page_last               o297
_journal_paper_doi               10.1107/S1600536811000456
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C70 H100 O5, 0.5C H2 Cl2'
_chemical_formula_moiety         'C70 H100 O5, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C70.5 H101 Cl O5'
_chemical_formula_weight         1064.03
_chemical_name_systematic
;
5,11,17,23,29-Penta-<i>tert</i>-butyl-31,32,33,34,35-pentapropoxycalix[5]arene
dichloromethane hemisolvate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.7460(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3740(2)
_cell_length_b                   23.9130(2)
_cell_length_c                   43.6550(5)
_cell_measurement_reflns_used    390743
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      1.00
_cell_volume                     12911.5(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'CRYSTALS (Betteridge <i>et al.</i>, 2003) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            39073
_diffrn_reflns_theta_full        24.105
_diffrn_reflns_theta_max         24.105
_diffrn_reflns_theta_min         1.263
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.88
_refine_diff_density_min         -1.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1531
_refine_ls_number_reflns         20282
_refine_ls_number_restraints     220
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.0004450
_refine_ls_shift/su_mean         5.2493401
_refine_ls_structure_factor_coef Fsqd
_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:
 11.5 14.0 3.91
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1509
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                13395
_reflns_number_total             20282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5077.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C70.5 H101 Cl1 O5'
_cod_database_code               2229223
_cod_database_fobs_code          2229223