X-ray diffraction and 13C solid-state NMR studies of the solvate of tetra(C-undecyl)calix[4]resorcinarene with dimethylacetamide
Kuzmicz, Rafal; Dobrzycki, Lukasz; Wozniak, Krzysztof; Benevelli, Francesca; Klinowski, Jacek; Kolodziejski, Waclaw; Physical Chemistry Chemical Physics 4 (2002) 2387–2391; doi:10.1039/b107416b

data_7204893
_publ_section_title
;
 X-ray diffraction and 13C solid-state NMR studies of the solvate of
 tetra(C-undecyl)calix[4]resorcinarene with dimethylacetamide
;
_journal_coden_ASTM              PPCPFQ
_journal_issue                   11
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              2387
_journal_page_last               2391
_journal_paper_doi               10.1039/b107416b
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C92 H157 N5 O13'
_chemical_formula_weight         1541.29
_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                78.31(3)
_cell_angle_beta                 89.92(3)
_cell_angle_gamma                77.10(3)
_cell_formula_units_Z            2
_cell_length_a                   9.773(2)
_cell_length_b                   17.050(3)
_cell_length_c                   27.745(6)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      4
_cell_volume                     4408.3(17)
_computing_cell_refinement       CrysAlisRED
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       omega_scan
_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  0.1538
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42505
_diffrn_reflns_theta_full        20.50
_diffrn_reflns_theta_max         20.50
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        1%
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  1500_sec
_diffrn_standards_number         1_frame
_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_T_max  -
_exptl_absorpt_correction_T_min  -
_exptl_absorpt_correction_type   -
_exptl_absorpt_process_details   -
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         8791
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.1171
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2888
_refine_ls_wR_factor_ref         0.3412
_reflns_number_gt                4500
_reflns_number_total             8802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cryst_data.txt
_cod_data_source_block           CAV11xDMA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not mesured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4408.7(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204893