Ketone transformation as a pathway to inherently chiral rigidified calix[4]arenes.
Tlustý, Martin; Spálovská, Dita; Kohout, Michal; Eigner, Václav; Lhoták, Pavel; Chemical communications (Cambridge, England) 56 (2020) 12773–12776; doi:10.1039/d0cc05352j

data_7127248
_publ_section_title
;
 Ketone transformation as a pathway to inherently chiral rigidified
 calix[4]arenes.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12773
_journal_page_last               12776
_journal_paper_doi               10.1039/d0cc05352j
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H47 N1 O5'
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_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4753(3)
_cell_length_b                   19.0877(5)
_cell_length_c                   39.5036(11)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    200
_cell_measurement_theta_max      47.67
_cell_measurement_theta_min      2.23
_cell_volume                     7144.7(4)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_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      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
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_diffrn_reflns_av_unetI/netI     0.084
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_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            41962
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_diffrn_reflns_theta_max         68.403
_diffrn_reflns_theta_min         2.237
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_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2720.029
_exptl_crystal_size_max          0.486
_exptl_crystal_size_mid          0.172
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_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 4824 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.27(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9219
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         12632
_refine_ls_number_restraints     183
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.0005095
_refine_ls_shift/su_mean         0.0000456
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 8.23P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1564
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1564
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              43
_reflns_limit_l_min              -47
_reflns_number_gt                11723
_reflns_number_total             12633
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.61
_oxford_diffrn_Wilson_scale      479.15
_oxford_refine_ls_r_factor_ref   0.0658
_oxford_refine_ls_scale          0.053937(9)
_oxford_reflns_number_all        12632
_cod_data_source_file            d0cc05352j2.cif
_cod_data_source_block           7
_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 7127245--7127248.cif.
;
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C41 H47 N1 O5'
_cod_database_code               7127248
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0658
_oxford_refine_ls_wr_factor_all  0.1564
_oxford_hooft_y                  0.27(8)
_oxford_bijvoet_difference       0.27(7)
_oxford_refined_flack_x          0.2(2)