Three conformational polymorphs and order‒disorder phase transition in a calix[4]arene bis(crown)
Thuéry, Pierre; Nierlich, Martine; Calemczuk, Roberto; Saadioui, Mohamed; Asfari, Zouhair; Vicens, Jacques; Acta Crystallographica Section B 55 (1999) 95–103; doi:10.1107/S0108768198009252

data_2105530
_publ_section_title
;
 Three conformational polymorphs and order--disorder phase transition in a
 calix[4]arene bis(crown)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              95
_journal_page_last               103
_journal_paper_doi               10.1107/S0108768198009252
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C58 H64 N2 O12'
_chemical_formula_weight         981.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.72(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.667(4)
_cell_length_b                   18.647(11)
_cell_length_c                   20.188(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     5144(4)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1993)'
_computing_publication_material  'SHELXTL (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .02
_diffrn_reflns_av_sigmaI/netI    .0617
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6514
_diffrn_reflns_theta_max         22
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        4.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          .70
_exptl_crystal_size_mid          .60
_exptl_crystal_size_min          .50
_refine_diff_density_max         1.493
_refine_diff_density_min         -.597
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.363
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.170
_refine_ls_restrained_S_obs      1.369
_refine_ls_R_factor_all          .2004
_refine_ls_R_factor_obs          .1273
_refine_ls_shift/esd_max         .019
_refine_ls_shift/esd_mean        .007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+16.0150P], where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .3850
_refine_ls_wR_factor_obs         .3155
_reflns_number_observed          2449
_reflns_number_total             6301
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            an0547.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+16.0150P], where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+16.0150P], where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5145(4)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2105530