Intra- and Intermolecular Hydrogen Bonding in a Tetrahydroxycalix[4]arene
Böhmer, V.; Ferguson, G.; Grüttner, C.; Vogt, W.; Acta Crystallographica Section C 53 (1997) 469–472; doi:10.1107/S0108270196015508

data_2006026
_publ_section_title
;
 Intra- and Intermolecular Hydrogen Bonding in a
 Tetrahydroxycalix[4]arene
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              469
_journal_page_last               472
_journal_paper_doi               10.1107/S0108270196015508
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C45 H49 N O6, 0.5C H Cl3 '
_chemical_formula_sum            'C45.5 H49.5 Cl1.5 N O6'
_chemical_formula_weight         759.54
_chemical_name_systematic
;
11,17-Di-tert-butyl-25,26,27,28-tetrahydroxy-2,5,23-trimethyl-14-(4-nitro-
phenyl)calix[4]arene Hemichloroform Solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                101.622(8)
_cell_angle_beta                 104.206(10)
_cell_angle_gamma                99.248(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3121(12)
_cell_length_b                   13.9765(12)
_cell_length_c                   14.973(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      17.40
_cell_measurement_theta_min      5.60
_cell_volume                     1998.3(4)
_computing_cell_refinement       'SET4 and CELDIM (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD-4/PC (Enraf-Nonius, 1992)'
_computing_data_reduction
'DATRD2  NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
'NRCVAX94, ORTEPII (Johnson, 1976), PLATON (Spek, 1996a), PLUTON (Spek 1996b)'
_computing_publication_material
'NRCVAX94, SHELXL93  and WordPerfect macro PREPCIF (Ferguson, 1996)'
_computing_structure_refinement  'NRCVAX94 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.2294
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6962
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        '0%, variation 1.0'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'very pale yellow'
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.290
_refine_ls_extinction_coef       0.0070(13)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.847
_refine_ls_goodness_of_fit_obs   1.256
_refine_ls_hydrogen_treatment    'H atoms riding (C-H 0.93-0.98, O-H 0.82\%A)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         6962
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.849
_refine_ls_restrained_S_obs      1.253
_refine_ls_R_factor_all          0.2328
_refine_ls_R_factor_obs          0.0536
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1803
_refine_ls_wR_factor_obs         0.1323
_reflns_number_observed          2071
_reflns_number_total             6962
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1430.cif
_cod_data_source_block           9488
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0871P)^2^] 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^)+(0.0871P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C45.50 H49.50 Cl1.50 N O6'
_cod_database_code               2006026