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_7224816
_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         'C60 H80 N4 O6'
_chemical_formula_sum            'C60 H80 N4 O6'
_chemical_formula_weight         953.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-18T19:55:04-00:00
_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                90
_cell_angle_beta                 109.896(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0623(5)
_cell_length_b                   21.8364(3)
_cell_length_c                   25.8796(5)
_cell_measurement_reflns_used    28947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4714
_cell_measurement_theta_min      2.8037
_cell_volume                     11192.2(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0023451
_diffrn_orient_matrix_UB_12      0.001595
_diffrn_orient_matrix_UB_13      0.0279822
_diffrn_orient_matrix_UB_21      0.0353328
_diffrn_orient_matrix_UB_22      0.0047181
_diffrn_orient_matrix_UB_23      0.0078138
_diffrn_orient_matrix_UB_31      -0.005355
_diffrn_orient_matrix_UB_32      0.0320879
_diffrn_orient_matrix_UB_33      -0.0025528
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            145617
_diffrn_reflns_theta_full        32
_diffrn_reflns_theta_max         32
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99626
_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            colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         38570
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.07
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.4216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                29868
_reflns_number_total             38570
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6ra05865e2.cif
_cod_data_source_block           modd268
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_database_code               7224816