Assembly modes in the solid state structure of the complexes of melamine mono-cations with para-calix[4]arene sulfonic acid and calix[4]arene dihydroxyphosphonic acid
Lazar, Adina N.; Danylyuk, Oksana; Suwinska, Kinga; Coleman, Anthony W.; New Journal of Chemistry 30 (2006) 59–; doi:10.1039/b510232b

data_7051516
_publ_section_title
;
 Assembly modes in the solid state structure of the complexes of
 melamine mono-cations with para-calix[4]arene sulfonic acid and
 calix[4]arene dihydroxyphosphonic acid
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              59
_journal_paper_doi               10.1039/b510232b
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C40 H66 N24 O28.5 S4'
_chemical_formula_weight         1467.41
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.286(4)
_cell_angle_beta                 86.453(4)
_cell_angle_gamma                82.786(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1991(6)
_cell_length_b                   15.2930(10)
_cell_length_c                   19.0080(10)
_cell_measurement_reflns_used    7527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      2.546
_cell_volume                     3122.2(3)
_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_molecular_graphics    'ORTEP-3 (Johnson & Burnet, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean
;
1242 (horizontal) x 1152 (vertical) pixels, CCD pixel size is 22.5 x 22.5 \mm
which gives at the input a pixel of 110 x 110 \mm (with 2 x 2 binning)
;
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method
;
395 frames via \w rotation
(rotation angle 0.9\% and 2*369 s per frame)
;
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27163
_diffrn_reflns_theta_full        22.02
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0022(4)
_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   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+3.4921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                5385
_reflns_number_total             7510
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b510232b.txt
_cod_data_source_block           para-sulphonato_calix[4]arene.melamine
_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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3122.3(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C40 H66 N24 O28.50 S4'
_cod_database_code               7051516