Nitration of thiacalix[4]arene using nitrosium nitrate complexes: synthesis and characterization of tetranitro-, tetraamino-, and tetra(4-pyridylimino)tetrahydroxythiacalix[4]arene
Desroches, Cédric; Parola, Stéphane; Vocanson, Francis; Perrin, Monique; Lamartine, Roger; Létoffé, Jean-Marie; Bouix, Jean; New Journal of Chemistry 26 (2002) 651–; doi:10.1039/b110609k

data_7050789
_publ_section_title
;
 Nitration of thiacalix[4]arene using nitrosium nitrate complexes:
 synthesis and characterization of tetranitro-, tetraamino-, and
 tetra(4-pyridylimino)tetrahydroxythiacalix[4]arene
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              651
_journal_paper_doi               10.1039/b110609k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C28 H24 N4 O14 S6'
_chemical_formula_weight         832.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.27(3)
_cell_angle_beta                 107.02(3)
_cell_angle_gamma                113.53(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2988(17)
_cell_length_b                   9.1492(18)
_cell_length_c                   12.431(3)
_cell_measurement_temperature    173(2)
_cell_volume                     811.0(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5948
_diffrn_reflns_theta_full        27.28
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.8325
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                2198
_reflns_number_total             3462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110609k.txt
_cod_data_source_block           cd
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        811.0(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050789