Synthesis, characterization and optical power limiting behaviour of phenylazo- and 4-nitrophenylazo-tetrahydroxytetrathiacalix[4]arene
Cédric Desroches; Stéphane Parola; Francis Vocanson; Noëlle Ehlinger; Philippe Miele; Roger Lamartine; Jean Bouix; Anders Eriksson; Mikael Lindgren; Cesar Lopes; J. Mater. Chem. 11 () 3014–3017; doi:10.1039/b105034f

data_7204174
_publ_section_title
;
 Synthesis, characterization and optical power limiting behaviour of
 phenylazo- and 4-nitrophenylazo-tetrahydroxytetrathiacalix[4]arene
;
_journal_issue                   12
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              3014
_journal_page_last               3017
_journal_paper_doi               10.1039/b105034f
_journal_volume                  11
_chemical_formula_sum            'C83 H63 N19 O12 S4'
_chemical_formula_weight         1646.76
_chemical_name_common
;
p-tetrakis(4-nitrophenylazo)-tetrahydroxythiacalix[4]arene
;
_chemical_name_systematic
;
p-tetrakis(4-nitrophenylazo)-tetrahydroxythiacalix[4]arene
;
_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                65.773(2)
_cell_angle_beta                 70.237(2)
_cell_angle_gamma                88.749(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7076(5)
_cell_length_b                   13.6925(5)
_cell_length_c                   15.3195(6)
_cell_measurement_reflns_used    21779
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1909.62(14)
_computing_cell_refinement       Denzo
_computing_data_collection       'Denzo (Otwinowski & Minor 1997)'
_computing_data_reduction        Denzo
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Nonius CCD'
_diffrn_measurement_method       'area detector'
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14905
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.8946
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.7827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                4437
_reflns_number_total             8717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105034f.txt
_cod_data_source_block           azo4s
_cod_database_code               7204174