Systematic Structural Coordination Chemistry of p-tert-Butyltetrathiacalix[4]arene: 1. Group 1 Elements and Congeners
Alexander Bilyk; Annegret K. Hall; Jack M. Harrowfield; M. Wais Hosseini; Brian W. Skelton; Allan H. White; Inorganic Chemistry 40 (2001) 672–686; doi:10.1021/ic001008c

data_4319255
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   Nedlands
   Western Australia 6907
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
 Systematic Structural Coordination Chemistry of
 p-tert-Butyltetrathiacalix[4]arene: 1. Group 1 Elements and Congeners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              672
_journal_page_last               686
_journal_paper_doi               10.1021/ic001008c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C48 H69 N O5 S5'
_chemical_formula_weight         900.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 96.025(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   14.4600(10)
_cell_length_b                   16.153(2)
_cell_length_c                   21.147(2)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.4
_cell_volume                     4912.1(8)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .031
_diffrn_reflns_av_sigmaI/netI    .068
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            72516
_diffrn_reflns_theta_max         34.01
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .28
_exptl_absorpt_correction_T_max  .94
_exptl_absorpt_correction_T_min  .80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .12
_refine_diff_density_max         .73
_refine_diff_density_min         -.394
_refine_ls_goodness_of_fit_all   1.19
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     846
_refine_ls_number_reflns         13681
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .064
_refine_ls_R_factor_gt           .04
_refine_ls_shift/su_max          .091
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .051
_refine_ls_wR_factor_ref         .047
_reflns_d_resolution_high        .635
_reflns_d_resolution_low         12.778
_reflns_Friedel_coverage         0
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              -33
_reflns_number_gt                13681
_reflns_number_total             18664
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            ic001008c_09.cif
_cod_data_source_block           mgs4
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_formula_sum        'C48 H69 N1 O5 S5'
_cod_database_code               4319255