5,11,17,23-Tetrakis(chloromethyl)-25,26,27,28-tetrapropoxycalix[4]arene
Kutter, Felix; Düker, Matthias H.; Zeller, Matthias; Azov, Vladimir A.; Acta Crystallographica Section E 67 (2011) o728–o729; doi:10.1107/S160053681100660X

data_2229490
_publ_section_title
;
 5,11,17,23-Tetrakis(chloromethyl)-25,26,27,28-tetrapropoxycalix[4]arene
;
_journal_coeditor_code           RK2266
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o728
_journal_page_last               o729
_journal_paper_doi               10.1107/S160053681100660X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C44 H52 Cl4 O4'
_chemical_formula_moiety         'C44 H52 Cl4 O4'
_chemical_formula_sum            'C44 H52 Cl4 O4'
_chemical_formula_weight         786.66
_chemical_melting_point_gt       562
_chemical_melting_point_lt       565
_chemical_name_systematic
;
5,11,17,23-Tetrakis(chloromethyl)-25,26,27,28-tetrapropoxycalix[4]arene
;
_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
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 117.655(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.104(3)
_cell_length_b                   11.5871(15)
_cell_length_c                   17.618(2)
_cell_measurement_reflns_used    6719
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.16
_cell_measurement_theta_min      2.61
_cell_volume                     4177.7(9)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2009)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2009)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2009)'
_computing_molecular_graphics
;
<i>ORTEP-3</i> (Farrugia, 1997) and <i>Mercury</i> (Macrae <i>et
al.</i>,
2006)
;
_computing_publication_material
;
<i>CRYSTALS</i> (Betteridge <i>et al.</i>, 2003), <i>enCIFer</i>
(Allen <i>et al.</i>, 2004) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>CRYSTALS</i> (Betteridge <i>et al.</i>, 2003)
;
_computing_structure_solution    '<i>SIR97</i> (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine--focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15796
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         31.310
_diffrn_reflns_theta_min         1.990
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9738
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.0009018
_refine_ls_shift/su_mean         0.1538122
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method: Modified Sheldrick
w=1/[\s^2^(F^2^)+(0.06P)^2^+6.50P], where P=(max(Fo^2^,0)+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1188
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                5280
_reflns_number_total             6176
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2266.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229490
_cod_database_fobs_code          2229490