Cone and 1,3-alternate conformers of 1,3-bis(ethoxycarbonylmethoxy)-2,4-dihydroxycalix[4]arene and 1,2,3,4-tetrakis(ethoxycarbonylmethoxy)calix[4]arene
Genorio, Boštjan; Kobe, Jože; Giester, Gerald; Leban, Ivan; Acta Crystallographica Section C 59 (2003) o221–o224; doi:10.1107/S0108270103005298

data_2013323
_publ_section_title
;
 Cone and 1,3-alternate conformers of
 1,3-bis(ethoxycarbonylmethoxy)-2,4-dihydroxycalix[4]arene and
 1,2,3,4-tetrakis(ethoxycarbonylmethoxy)calix[4]arene
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o221
_journal_page_last               o224
_journal_paper_doi               10.1107/S0108270103005298
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C44 H48 O12'
_chemical_formula_moiety         'C44 H48 O12'
_chemical_formula_sum            'C44 H48 O12'
_chemical_formula_weight         768.82
_chemical_melting_point          109.0(10)
_chemical_name_common
;
1,2,3,4-tetrakis(methoxycarbonylethoxy)calix[4]arene
;
_chemical_name_systematic
;
tetraethyl calix[4]arene-1,2,3,4-tetrayltetra(oxyacetate)
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   12.0173(8)
_cell_length_b                   12.0173(8)
_cell_length_c                   7.6972(5)
_cell_measurement_reflns_used    5413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1111.59(13)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1999)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEPII (Johnson, 1971), PLUTON (Spek, 1991),
PLATON (Spek, 2003; Farrugia, 2000),
ORTEP-3 (Farrugia, 1997), MERCURY (Bruno et al., 2002)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 1997), PARST (Nardelli, 1983 and 1995),
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.055
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method
;
\w scans
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2991
_diffrn_reflns_theta_full        29.19
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         5.37
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      1.10(5)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.232
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0647
_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^)+(0.1240P)^2^+0.2336P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                1453
_reflns_number_total             1604
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1598.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '108-110' was changed to '109.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '108-110' was changed to '109.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1111.60(13)
_cod_original_sg_symbol_H-M      P-4
_cod_database_code               2013323
_cod_database_fobs_code          2013323