A tetra-<i>tert</i>-butylcalix[4]arene-12-crown-4 <i>N,N</i>-dimethylformamide inclusion complex
Jeffrey C. Bryan; Tatiana G. Levitskaia; Acta Crystallographica Section E 58 (2002) o240–o242; doi:10.1107/S1600536802002076

data_2200966
_publ_section_title
;
 A tetra-<i>tert</i>-butylcalix[4]arene-12-crown-4
 <i>N,N</i>-dimethylformamide inclusion complex
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o240
_journal_page_last               o242
_journal_paper_doi               10.1107/S1600536802002076
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C50 H66 O6, C3 H7 N O'
_chemical_formula_structural     'C50 H66 O6, C3 H7 N O'
_chemical_formula_sum            'C53 H73 N O7'
_chemical_formula_weight         836.1
_chemical_name_common
;
tetra-t-butylcalix[4]arene-1,2-crown-4 N,N-dimethylformamide
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.087(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6115(13)
_cell_length_b                   20.000(3)
_cell_length_c                   19.995(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      10.0
_cell_volume                     4820.7(12)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_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  .022
_diffrn_reflns_av_sigmaI/netI    .069
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10485
_diffrn_reflns_reduction_process
;
XCAD4 (Harms, 1995)
;
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          .47
_exptl_crystal_size_mid          .41
_exptl_crystal_size_min          .34
_refine_diff_density_max         .66
_refine_diff_density_min         -.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8451
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          .119
_refine_ls_R_factor_gt           .058
_refine_ls_shift/su_max          .00
_refine_ls_shift/su_mean         .00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0742P)^2^+3.2092P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .146
_refine_ls_wR_factor_ref         .171
_reflns_number_gt                5151
_reflns_number_total             8451
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6080.cif
_cod_data_source_block           I
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2200966
_cod_database_fobs_code          2200966