Synthesis, structure and conformational mobility of tetra-substituted cyanomethoxy p-tert-butylcalix[4]arenes
D'Alessio, Daniel; Krause-Heuer, Answen M; Skelton, Brian W.; Fraser, Benjamin Hugh; Massi, Massimiliano; Ogden, Mark Ian; RSC Adv.  (2016) –; doi:10.1039/C6RA05865E

data_7224819
_publ_section_title
;
 Synthesis, structure and conformational mobility of tetra-substituted
 cyanomethoxy p-tert-butylcalix[4]arenes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA05865E
_journal_year                    2016
_chemical_formula_moiety         'C56 H70 N4 O5, C2 H6 O'
_chemical_formula_sum            'C58 H76 N4 O6'
_chemical_formula_weight         925.23
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-09T21:51:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-02-29 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                81.960(4)
_cell_angle_beta                 79.731(4)
_cell_angle_gamma                84.962(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6671(5)
_cell_length_b                   12.4238(5)
_cell_length_c                   21.0581(9)
_cell_measurement_reflns_used    9118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4873
_cell_measurement_theta_min      2.8082
_cell_volume                     2713.4(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0406699
_diffrn_orient_matrix_UB_12      -0.033915
_diffrn_orient_matrix_UB_13      -0.0204086
_diffrn_orient_matrix_UB_21      0.0002348
_diffrn_orient_matrix_UB_22      -0.0417484
_diffrn_orient_matrix_UB_23      0.0266324
_diffrn_orient_matrix_UB_31      -0.0541692
_diffrn_orient_matrix_UB_32      -0.0210042
_diffrn_orient_matrix_UB_33      -0.0079726
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.055
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32902
_diffrn_reflns_theta_full        29
_diffrn_reflns_theta_max         29
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.87277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
      CrysAlisPro, Oxford Diffraction Ltd.,
  Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14427
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+1.7596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2064
_reflns_number_gt                10878
_reflns_number_total             14427
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6ra05865e2.cif
_cod_data_source_block           modd274
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7224819