Solid state structures of the complexes between the antiseptic chlorhexidine and three anionic derivatives of calix[4]arene
Dupont, Nathalie; Lazar, Adina N.; Perret, Florent; Danylyuk, Oksana; Suwinska, Kinga; Navaza, Alda; Coleman, Anthony W.; CrystEngComm 10 (2008) 975–; doi:10.1039/b805317k

data_7202141
_publ_section_title
;
 Solid state structures of the complexes between the antiseptic
 chlorhexidine and three anionic derivatives of calix[4]arene
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              975
_journal_paper_doi               10.1039/b805317k
_journal_volume                  10
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_moiety
;
C22 H33 Cl2 N10, C28 H20 O16 S4,3(C1 H4 O1), 6(H2 O1)
;
_chemical_formula_sum            'C53 H77 Cl2 N10 O25 S4'
_chemical_formula_weight         1453.39
_chemical_name_common            'para-sulfonatocalix(4)arene Chlorhexidine'
_chemical_name_systematic        'para-sulfonatocalix[4]arene Chlorhexidine'
_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                65.687(2)
_cell_angle_beta                 77.180(2)
_cell_angle_gamma                64.4270(10)
_cell_formula_units_Z            2
_cell_length_a                   15.3260(5)
_cell_length_b                   15.9820(5)
_cell_length_c                   16.1350(4)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.95
_cell_volume                     3244.08(18)
_computing_cell_refinement
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_collection
'Collect data collection software (Nonius B.V., 1998)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       rotation
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17554
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             1526
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
'About three disordered methanol molecules were squeezed'
;
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0028(5)
_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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         9255
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+3.8457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                6813
_reflns_number_total             9255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805317k.txt
_cod_data_source_block           Calix[4]sulfonateChlorhexidine
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3244.08(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202141