Interplay between cone and partial-cone geometry in doubly-bridged calix[8]arenes investigated by X-ray and 2D NMR
Geraci, Corrada; Bottino, Alessandra; Piattelli, Mario; Gavuzzo, Enrico; Neri, Placido; Journal of the Chemical Society, Perkin Transactions 2  (2000) 185–; doi:10.1039/a909410e

data_7203955
_publ_section_title
;
 Interplay between cone and partial-cone geometry in doubly-bridged
 calix[8]arenes investigated by X-ray and 2D NMR
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              185
_journal_paper_doi               10.1039/a909410e
_journal_year                    2000
_chemical_formula_sum            'C97 H130 Cl2 O10'
_chemical_formula_weight         1527.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_cell_angle_alpha                108.700
_cell_angle_beta                 103.600
_cell_angle_gamma                72.700
_cell_formula_units_Z            2
_cell_length_a                   17.739
_cell_length_b                   21.050
_cell_length_c                   16.878
_cell_measurement_radiation      CuK\a
_cell_measurement_temperature    293
_cell_measurement_wavelength     1.54178
_cell_volume                     5631.073
_computing_molecular_graphics
'SIR97(Altomare al.,J. Appl. Cryst.,1999,32,115)'
_computing_publication_material
'SIR97(Altomare al.,J. Appl. Cryst.,1999,32,115)'
_computing_structure_refinement
'SIR97(Altomare al.,J. Appl. Cryst.,1999,32,115)'
_computing_structure_solution
'SIR97(Altomare al.,J. Appl. Cryst.,1999,32,115)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'MSC-AFC5 Diffractometer'
_diffrn_measurement_method       w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_theta_max         62.12
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  no
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   'empirical via \y scans (TEXSAN,1985)'
_exptl_crystal_density_diffrn    0.901
_exptl_crystal_F_000             1652
_refine_diff_density_max         2.081
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    'H atoms rigid to parent C atom'
_refine_ls_matrix_type           diagonal
_refine_ls_number_parameters     965
_refine_ls_number_reflns         7350
_refine_ls_R_factor_all          0.147
_refine_ls_R_factor_obs          0.147
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     W=(Sin(Theta)/Lambda)^2
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.154
_refine_ls_wR_factor_obs         0.154
_reflns_d_resolution_high        0.872
_reflns_d_resolution_low         16.733
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              -22
_reflns_limit_l_max              18
_reflns_limit_l_min              -19
_reflns_number_observed          7350
_reflns_number_total             17748
_reflns_observed_criterion       ' F >6.0 sigma(F) '
_cod_data_source_file            a909410e.txt
_cod_data_source_block           global
_cod_depositor_comments
;
 Updating the _atom_site_label, _atom_site_aniso_label and _atom_type_symbol
 data item values to establish relationships between rows in different loops.

 Antanas Vaitkus,
 2018-08-02

 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2018-08-02

 Changing the space group from 'P 1' to 'P -1' after consulting the original
 publication.

 Antanas Vaitkus,
 2018-08-02

The following automatic conversions were performed:
'_refine_ls_matrix_type' value 'Diagonal' changed to 'diagonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_thermal_displace_type' value 'uiso' changed to
'Uiso' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (127
times).

'_atom_site_thermal_displace_type' value 'uani' changed to 'Uani'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (104 times).

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 'W=(Sin(Theta)/Lambda)^2' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'W=(Sin(Theta)/Lambda)^2'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'p -1'
_cod_original_formula_sum        H130C97O10Cl2
_cod_database_code               7203955