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_7056265
_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         'C80 H96 N8 O4,C H Cl3'
_chemical_formula_sum            'C81 H97 Cl3 N8 O4'
_chemical_formula_weight         1353.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-05-29 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.511(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9892(10)
_cell_length_b                   14.9268(12)
_cell_length_c                   24.0802(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      2.5
_cell_volume                     7461.3(9)
_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 0.958
_diffrn_measured_fraction_theta_max 0.810
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41422
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         30.114
_diffrn_reflns_theta_min         1.818
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         17812
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+6.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9594
_reflns_number_total             17812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01389b1.cif
_cod_data_source_block           e2739a
_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 
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_cod_database_code               7056265
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2014/6
_shelx_res_checksum              69864