A C-shaped p-sulfonatocalix[4]arene-based supermolecule exhibiting mutual-inclusion and bilayer insertion of dipicolinate
Husain, Ahmad; Oliver, Clive L.; CrystEngComm 16 (2014) 3749–; doi:10.1039/c3ce42358a

data_7214315
_publ_section_title
;
 A C-shaped p-sulfonatocalix[4]arene-based supermolecule exhibiting
 mutual-inclusion and bilayer insertion of dipicolinate
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3749
_journal_paper_doi               10.1039/c3ce42358a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'C84 H77 Ce3 N4 O61 S8, N O3, 7(H2 O), 14(O), 4(H O)'
_chemical_formula_sum            'C84 H95 Ce3 N5 O89 S8'
_chemical_formula_weight         3275.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 101.9030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8361(5)
_cell_length_b                   36.0691(12)
_cell_length_c                   23.6851(9)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.31
_cell_volume                     12402.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  'publCIF (Westrip, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       /w
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            106344
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.8776
_exptl_absorpt_correction_T_min  0.7753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.446
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1855
_refine_ls_number_reflns         21784
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+63.0734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                17074
_reflns_number_total             21784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42358a.txt
_cod_data_source_block           C:p21cfilled.CIF
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7214315