Alkali-Metalated Forms of Thiacalix[4]arenes
Zeller, Jürgen; Radius, Udo; Inorganic Chemistry 45 (2006) 9487–9492; doi:10.1021/ic0613311

data_4333050
_publ_section_title
;
 Alkali-Metalated Forms of Thiacalix[4]arenes
;
_journal_issue                   23
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9487
_journal_page_last               9492
_journal_paper_doi               10.1021/ic0613311
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C70 H72 N6 Na4 O4 S4'
_chemical_formula_weight         1281.53
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.62(3)
_cell_angle_beta                 101.38(3)
_cell_angle_gamma                110.04(3)
_cell_formula_units_Z            2
_cell_length_a                   14.513(3)
_cell_length_b                   15.335(3)
_cell_length_c                   17.759(4)
_cell_measurement_reflns_used    19925
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      56.46
_cell_measurement_theta_min      3.05
_cell_volume                     3413.3(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'stoe ipds 2'
_diffrn_measurement_method       rotation
_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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16183
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.9380
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         10554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                7842
_reflns_number_total             10554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613311sup3.cif
_cod_data_source_block           jzna
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C140 H144 N12 Na8 O8 S8'
_cod_original_formula_weight         2563.07
_cod_original_formula_units_Z            1
_cod_original_cell_volume        3413.1(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333050