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_7051517
_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            'C39 H68 N18 O20 P2'
_chemical_formula_weight         1171.05
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.281(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1727(9)
_cell_length_b                   12.4313(7)
_cell_length_c                   19.5080(10)
_cell_measurement_reflns_used    6715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      2.910
_cell_volume                     5233.3(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method
;
241 frames via \f rotation and 52 frames via \w rotation
(rotation angle 1.5\% and 2*300 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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.1185
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55429
_diffrn_reflns_theta_full        21.98
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9522
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.00187(19)
_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   1.005
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.143
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                4206
_reflns_number_total             6336
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b510232b.txt
_cod_data_source_block           calix[4]arene_dihydrophosphonic_acid.melamine
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P21/c
_cod_database_code               7051517