The atropisomeric dynamic behaviour of symmetrical N-acylated amine-bridged calix[4]arenes
Tlustý, M.; Eigner, V.; Dvořáková, H.; Lhoták, P.; New Journal of Chemistry 46 (2022) 11774–11781; doi:10.1039/D2NJ01533A

data_7061515
_publ_section_title
;
 The atropisomeric dynamic behaviour of symmetrical N-acylated
 amine-bridged calix[4]arenes
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11774
_journal_page_last               11781
_journal_paper_doi               10.1039/D2NJ01533A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C47 H50 N2 O7'
_chemical_formula_sum            'C47 H50 N2 O7'
_chemical_formula_weight         754.92
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-03-09 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2849(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.46594(8)
_cell_length_b                   17.66158(14)
_cell_length_c                   23.8239(2)
_cell_measurement_reflns_used    22486
_cell_measurement_temperature    130
_cell_measurement_theta_max      67.62
_cell_measurement_theta_min      3.08
_cell_volume                     3982.91(6)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_unetI/netI     0.031
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40926
_diffrn_reflns_theta_full        66.297
_diffrn_reflns_theta_max         67.650
_diffrn_reflns_theta_min         3.115
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608.001
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9781
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         7138
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.0008173
_refine_ls_shift/su_mean         0.0000787
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0950
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6468
_reflns_number_total             7139
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.52
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0403
_oxford_refine_ls_scale          4.21(4)
_oxford_reflns_number_all        7139
_cod_data_source_file            d2nj01533a2.cif
_cod_data_source_block           7c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061515.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7061515
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0403
_oxford_refine_ls_wr_factor_all  0.0950