Pentaalkyl ester derivatives of p-benzylcalix[5]arene and p-tert-octylcalix[5]arene: synthesis, crystal structure and metal ion complexation
Arnaud-Neu, Françoise; Asfari, Zouhair; Souley, Bahari; Vicens, Jacques; Thuéry, Pierre; Nierlich, Martine; Journal of the Chemical Society, Perkin Transactions 2  (2000) 495–; doi:10.1039/a908336g

data_7203934
_publ_section_title
;
 Pentaalkyl ester derivatives of p-benzylcalix[5]arene and
 p-tert-octylcalix[5]arene: synthesis, crystal structure and metal ion
 complexation
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              495
_journal_paper_doi               10.1039/a908336g
_journal_year                    2000
_chemical_formula_sum            'C90 H90 O15'
_chemical_formula_weight         1411.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.147(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.065(2)
_cell_length_b                   15.1021(4)
_cell_length_c                   26.5383(12)
_cell_measurement_reflns_used    44818
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.35
_cell_volume                     15017.2(11)
_computing_cell_refinement       'HKL package (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius, 1997)'
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_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  0.129
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44818
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             6000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.153
_refine_ls_goodness_of_fit_obs   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         10383
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.253
_refine_ls_restrained_S_obs      1.182
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_obs          0.0876
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+90.0662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2369
_refine_ls_wR_factor_obs         0.1751
_reflns_number_observed          6723
_reflns_number_total             10531
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908336g.txt
_cod_data_source_block           118pt
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+90.0662P] 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^)+(0.0499P)^2^+90.0662P] 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        15017(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7203934