Synthesis, Structures, and Conformational Characteristics of Calixarene Monoanions and Dianions
Tracy A. Hanna; Lihua Liu; Alfredo M. Angeles-Boza; Xiaodi Kou; C. David Gutsche; Krzysztof Ejsmont; William H. Watson; Lev N. Zakharov; Christopher D. Incarvito; Arnold L. Rheingold; Journal of the American Chemical Society 125 (2003) 6228–6238; doi:10.1021/ja0289797

data_4113742
_publ_contact_author             'Tracy A. Hanna'
_publ_contact_author_email       T.Hanna@tcu.edu
_publ_section_title
;
 Synthesis, Structures, and Conformational Characteristics of Calixarene
 Monoanions and Dianions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6228
_journal_page_last               6238
_journal_paper_doi               10.1021/ja0289797
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C45 H45 Cs O9'
_chemical_formula_weight         862.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.693(2)
_cell_length_b                   20.271(3)
_cell_length_c                   24.076(3)
_cell_measurement_temperature    213(2)
_cell_volume                     7658.9(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1970
_diffrn_reflns_av_sigmaI/netI    0.1518
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27538
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.9549
_exptl_absorpt_correction_T_min  0.8237
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       'elongated p'
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .17
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00000(12)
_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   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1982
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          4.422
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+138.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2912
_reflns_number_gt                2095
_reflns_number_total             4396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0289797si20021230_042221_07.cif
_cod_data_source_block           15
_cod_original_cell_volume        7659.0(18)
_cod_database_code               4113742