Redetermination of 5,11,17,23-tetra-<i>tert</i>-butyl-25,27-di(ethoxycarbonylmethoxy)-26,28-dihydroxycalix[4]arene chloroform disolvate at low temperature
Bolte, Michael; Danila, Crenguta; Böhmer, Volker; Acta Crystallographica Section E 59 (2003) o533–o534; doi:10.1107/S1600536803006032

data_2202072
_publ_section_title
;Redetermination of
 5,11,17,23-tetra-<i>tert</i>-butyl-25,27-di(ethoxycarbonylmethoxy)-26,28-dihydroxycalix[4]arene
 chloroform disolvate at low temperature
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o533
_journal_page_last               o534
_journal_paper_doi               10.1107/S1600536803006032
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C52 H68 O8, 2C H Cl3'
_chemical_formula_moiety         'C52 H68 O8, 2C H Cl3'
_chemical_formula_sum            'C54 H70 Cl6 O8'
_chemical_formula_weight         1059.80
_chemical_name_systematic
;(5,11,17,23-Tetra-t-butyl-26,28-dihydroxy-25,27-bis(ethoxycarbonylmethoxy)-pen
tacyclo(19.3.1.1^3,7^.1^9,13^.1^15,19^)octacosa-1(25),3,5,7(28),9,11,13(27),15
,17,19(26),21,23-dodecaene)
 clathrate chloroform solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   17.7766(2)
_cell_length_b                   20.41080(10)
_cell_length_c                   32.0452(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.5
_cell_volume                     11627.11(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART CCD three-circle'
_diffrn_measurement_method       \w
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52500
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.9099
_exptl_absorpt_correction_T_min  0.8663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.909
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10229
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0945
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1605P)^2^+26.7478P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2619
_refine_ls_wR_factor_ref         0.2973
_reflns_number_gt                6797
_reflns_number_total             10229
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6213.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_database_code               2202072
_cod_database_fobs_code          2202072