Conformational behaviour and first crystal structures of a calix[4]arene featuring a laterally positioned carboxylic acid function in unsolvated and solvent-complexed forms
Gruber, Tobias; Gruner, Margit; Fischer, Conrad; Seichter, Wilhelm; Bombicz, Petra; Weber, Edwin; New Journal of Chemistry 34 (2010) 250–; doi:10.1039/b904489b

data_7053250
_publ_section_title
;
 Conformational behaviour and first crystal structures of a calix[4]arene
 featuring a laterally positioned carboxylic acid function in unsolvated
 and solvent-complexed forms
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              250
_journal_paper_doi               10.1039/b904489b
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C49 H64 O6, C2 H6 O, H2 O'
_chemical_formula_sum            'C51 H72 O8'
_chemical_formula_weight         813.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   23.887(5)
_cell_length_b                   17.151(3)
_cell_length_c                   12.429(3)
_cell_measurement_reflns_used    6721
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.34
_cell_volume                     5092.0(19)
_computing_cell_refinement       'SAINT-NT (Sheldrick, 2004)'
_computing_data_collection       'Kappa APEX 2 (Bruker-AXS)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38796
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1633P)^2^+3.0043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2411
_reflns_number_gt                3725
_reflns_number_total             4759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904489b.txt
_cod_data_source_block           mape4last
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5092.1(18)
_cod_database_code               7053250