Synthesis and structural analysis of mercaptothiacalix[4]arene
Rao, Photon; Hosseini, Mir Wais; Cian, André De; Fischer, Jean; Chemical Communications  (1999) 2169–; doi:10.1039/a906058h

data_7110669
_publ_section_title
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 Synthesis and structural analysis of mercaptothiacalix[4]arene
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2169
_journal_paper_doi               10.1039/a906058h
_journal_year                    1999
_chemical_formula_moiety         'C121 H139 Cl2 O S24'
_chemical_formula_sum            'C121 H139 Cl2 O S24'
_chemical_formula_weight         2449.90
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                84.044(2)
_cell_angle_beta                 80.888(2)
_cell_angle_gamma                78.386(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9058(4)
_cell_length_b                   18.8600(4)
_cell_length_c                   24.5600(7)
_cell_measurement_reflns_used    49745
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      1.4
_cell_volume                     6659.2(3)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  49745 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  40. mm.
 Scan angle =  1.8 deg 1 scans of   54 sec per frame.
 Data collection was divided into  3 sets
 with the following starting angles and number of frames :

 Set 1 Theta =    9.94 Omega =  180.00 Kappa =    0.00  101 frames
 Set 2 Theta =   -5.49 Kappa = -173.12 Phi   =  163.54   24 frames
 Set 3 Theta =   -9.87 Kappa =   82.79 Phi   =  183.25   45 frames
 Friedel pairs were not averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            49745
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2582
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.386
_refine_diff_density_min         -0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   5.885
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         12582
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.194
_refine_ls_R_factor_gt           0.076
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.011
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+1.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.353
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                12582
_reflns_number_total             31535
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            906058hsup1.cif
_cod_data_source_block           st425
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+1.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+1.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        6659.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110669