(5,11,17,23-Tetra-<i>tert</i>-butyl-26,28-dihydroxycalix[4]arene-25,27-dioxy)diacetic acid <i>N</i>,<i>N</i>-dimethylformamide trisolvate
Schlientz, Leah M.; Hagen, Karl S.; Acta Crystallographica Section C 60 (2004) o533–o535; doi:10.1107/S010827010401323X

data_2014183
_publ_section_title
;(5,11,17,23-Tetra-<i>tert</i>-butyl-26,28-dihydroxycalix[4]arene-25,27-dioxy)diacetic
 acid <i>N</i>,<i>N</i>-dimethylformamide trisolvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o533
_journal_page_last               o535
_journal_paper_doi               10.1107/S010827010401323X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C48 H60 O8 , 3C3 H7 N O'
_chemical_formula_moiety         'C48 H60 O8 , 3C3 H7 N O'
_chemical_formula_sum            'C57 H81 N3 O11'
_chemical_formula_weight         984.25
_chemical_name_common            t-butyl-Calix[4]arene-diacid
_chemical_name_systematic
;(5,11,17,23-Tetra-tert-butyl-26,28-dihydroxycalix[4]arene-25,27-dioxy)diacetic
acid
 N,N-dimethylformamide trisolvate
;
_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                90.00
_cell_angle_beta                 96.991(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3624(3)
_cell_length_b                   35.2240(10)
_cell_length_c                   13.7180(4)
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      131.9
_cell_measurement_theta_min      5.0
_cell_volume                     5449.5(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25773
_diffrn_reflns_theta_full        66.19
_diffrn_reflns_theta_max         66.19
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.9607
_exptl_absorpt_correction_T_min  0.8621
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'face-indexing of crystal Reference'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                6845
_reflns_number_total             9142
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hj1009.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 

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 
;
_cod_original_cell_volume        5449.6(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2014183
_cod_database_fobs_code          2014183