Manipulating the conformation and interplay of p-sulfonated calix[4]arenes by lower rim tri-substitution with N′-cyanocarbamimidate groups
Ling, Irene; Skelton, Brian W.; Sobolev, Alexandre N.; Alias, Yatimah; Raston, Colin L.; CrystEngComm 16 (2014) 5159–; doi:10.1039/c4ce00336e

data_7215811
_publ_section_title
;
 Manipulating the conformation and interplay of p-sulfonated
 calix[4]arenes by lower rim tri-substitution with
 N&#x2032;-cyanocarbamimidate groups
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              5159
_journal_paper_doi               10.1039/c4ce00336e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C304 H496 Gd7 N80 Na7 O254 S32'
_chemical_formula_weight         11623.41
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 117.023(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   39.799(2)
_cell_length_b                   31.5266(9)
_cell_length_c                   22.9740(11)
_cell_measurement_reflns_used    4936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.822
_cell_volume                     25679(2)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-S, Sapphire3 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1131
_diffrn_reflns_av_sigmaI/netI    0.1532
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            100592
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.98196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             11898
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         2.845
_refine_diff_density_min         -3.404
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1798
_refine_ls_number_reflns         31123
_refine_ls_number_restraints     692
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.2253
_refine_ls_R_factor_gt           0.1420
_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^)+(0.0800P)^2^+450.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2837
_refine_ls_wR_factor_ref         0.3217
_reflns_number_gt                16365
_reflns_number_total             31123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00336e1.cif
_cod_data_source_block           210808b
_cod_depositor_comments          'Adding full bibliography for 7215811.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7215811