Synthesis of para- and meta-imino- or -amino-methyl pyridyl appended p-tert-butyl-calix[4]arene or p-tert-butyl-thiacalix[4]arene in 1,3-Alternate conformation
Noamane, Mohamed Habib; FERLAY, Sylvie; Abidi, Rym; Kyritsakas, Nathalie; Hosseini, Mir Wais; New J. Chem. 41 (2017) 6334–6339; doi:10.1039/C7NJ01389B

data_7056266
_publ_section_title
;
 Synthesis of para- and meta-imino- or -amino-methyl pyridyl appended
 p-tert-butyl-calix[4]arene or p-tert-butyl-thiacalix[4]arene in
 1,3-Alternate conformation
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_journal_issue                   14
_journal_name_full               'New J. Chem.'
_journal_page_first              6334
_journal_page_last               6339
_journal_paper_doi               10.1039/C7NJ01389B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C76 H96 N8 O4 S4'
_chemical_formula_sum            'C76 H96 N8 O4 S4'
_chemical_formula_weight         1313.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.689(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0334(16)
_cell_length_b                   13.939(2)
_cell_length_c                   36.796(6)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      246
_cell_volume                     7641.3(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20663
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.086
_diffrn_reflns_theta_min         2.028
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         20663
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.2218
_refine_ls_R_factor_gt           0.1068
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2769
_refine_ls_wR_factor_ref         0.3205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7948
_reflns_number_total             20663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01389b1.cif
_cod_data_source_block           e2793a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7056266
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.991
_diffrn_reflns_v_r_equivalents   0.054
_shelxl_version_number           2014/6
_shelx_res_checksum              12726
_shelx_fab_checksum              72195