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_7224818
_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         'C50 H59 N3 O4'
_chemical_formula_sum            'C50 H59 N3 O4'
_chemical_formula_weight         766
_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             2012-02-21T14:03:57-00:00
_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                78.456(3)
_cell_angle_beta                 71.355(4)
_cell_angle_gamma                75.486(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2306(5)
_cell_length_b                   12.9547(5)
_cell_length_c                   16.8293(7)
_cell_measurement_reflns_used    7061
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9652
_cell_measurement_theta_min      2.8043
_cell_volume                     2226.64(17)
_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
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        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
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        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 0.994
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0192565
_diffrn_orient_matrix_UB_12      -0.0445174
_diffrn_orient_matrix_UB_13      -0.0230492
_diffrn_orient_matrix_UB_21      0.0631624
_diffrn_orient_matrix_UB_22      -0.0078596
_diffrn_orient_matrix_UB_23      0.0033082
_diffrn_orient_matrix_UB_31      -0.0164765
_diffrn_orient_matrix_UB_32      -0.0347893
_diffrn_orient_matrix_UB_33      0.0383646
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20351
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         29
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.97863
_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    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         11503
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.091
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.7801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                8528
_reflns_number_total             11503
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6ra05865e2.cif
_cod_data_source_block           modd233
_cod_original_cell_volume        2226.64(16)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7224818