Salt formation affects the conformational and assembly properties of p-carboxylatocalix[4]arenes
Kennedy, Stuart; Beavers, Christine M.; Teat, Simon J.; Dalgarno, Scott J.; CrystEngComm 16 (2014) 3712–; doi:10.1039/c3ce42523a

data_7214334
_publ_section_title
;
 Salt formation affects the conformational and assembly properties of
 p-carboxylatocalix[4]arenes
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3712
_journal_paper_doi               10.1039/c3ce42523a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C130.65 H167.3 N16 O34'
_chemical_formula_weight         2505.90
_chemical_name_common            methanolpropoxy
_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                87.763(4)
_cell_angle_beta                 84.240(4)
_cell_angle_gamma                77.864(3)
_cell_formula_units_Z            2
_cell_length_a                   16.5671(14)
_cell_length_b                   19.7029(17)
_cell_length_c                   20.3946(18)
_cell_measurement_temperature    100(2)
_cell_volume                     6474.5(10)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66296
_diffrn_reflns_theta_full        22.15
_diffrn_reflns_theta_max         22.15
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.9636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2670
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.155
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1760
_refine_ls_number_reflns         15780
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.898
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2542
_reflns_number_gt                12285
_reflns_number_total             15780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42523a2.cif
_cod_data_source_block           32AP
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C130.65 H167.30 N16 O34'
_cod_database_code               7214334