Solid-state and solution studies of bis-carboxylate binding by bis-amidinium calix[4]arenes†
Camiolo, Salvatore; Gale, Philip A.; Ogden, Mark I.; Skelton, Brian W.; White, Allan H.; Journal of the Chemical Society, Perkin Transactions 2  (2001) 1294–; doi:10.1039/b102831f

data_7216970
_publ_section_title
;
 Solid-state and solution studies of bis-carboxylate binding by
 bis-amidinium calix[4]arenes&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1294
_journal_paper_doi               10.1039/b102831f
_journal_year                    2001
_chemical_formula_sum            'C64.5 H83.5 N10 O20.25'
_chemical_formula_weight         1322.93
_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                86.248(6)
_cell_angle_beta                 89.449(6)
_cell_angle_gamma                85.085(6)
_cell_formula_units_Z            2
_cell_length_a                   11.256(4)
_cell_length_b                   12.126(5)
_cell_length_c                   24.781(9)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3363(2)
_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  .053
_diffrn_reflns_av_sigmaI/netI    .116
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37455
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .098
_exptl_absorpt_correction_T_max  .843
_exptl_absorpt_correction_T_min  .553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       prism
_exptl_crystal_F_000             1405
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .1
_refine_diff_density_max         .662
_refine_diff_density_min         -.498
_refine_ls_extinction_coef       1121(816)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.222
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     888
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .113
_refine_ls_R_factor_gt           .068
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .082
_refine_ls_wR_factor_ref         .072
_reflns_d_resolution_high        .73
_reflns_d_resolution_low         12.333
_reflns_Friedel_coverage         0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              33
_reflns_limit_l_min              -32
_reflns_number_gt                10356
_reflns_number_total             16219
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b102831f.txt
_cod_data_source_block           mo4gn
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C64.5 H83.5  N10 O20.25'
_cod_database_code               7216970