Design and synthesis of multifunctional thiacalixarenes and related metal derivatives for the preparation of sol‒gel hybrid materials with non-linear optical properties
Desroches, Cedric; Lopes, Cesar; Kessler, Vadim; Parola, Stephane; Dalton Transactions  (2003) 2085–2092; doi:10.1039/b210252h

data_7031144
_publ_section_title
;
 Design and synthesis of multifunctional thiacalixarenes and related metal
 derivatives for the preparation of sol--gel hybrid materials with
 non-linear optical properties
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              2085
_journal_page_last               2092
_journal_paper_doi               10.1039/b210252h
_journal_year                    2003
_chemical_formula_sum            'C88 H96 O4 S4'
_chemical_formula_weight         1345.89
_chemical_name_systematic        ?
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.796(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.009(4)
_cell_length_b                   23.370(4)
_cell_length_c                   17.968(3)
_cell_measurement_reflns_used    999(I>2sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.40
_cell_volume                     7837(3)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD 1k'
_diffrn_measurement_method       'Bruker SMART'
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11918
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00021(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                2045
_reflns_number_total             3654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210252h.txt
_cod_data_source_block           calix1tm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        7837(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7031144