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_7127246
_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_formula_moiety         'C41 H47 N O5, C2 H6 O'
_chemical_formula_sum            'C43 H53 N O6'
_chemical_formula_weight         679.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.3131(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1917(4)
_cell_length_b                   16.8403(5)
_cell_length_c                   18.4369(5)
_cell_measurement_reflns_used    114
_cell_measurement_temperature    250
_cell_measurement_theta_max      49
_cell_measurement_theta_min      13
_cell_volume                     3930.9(2)
_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      250
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59374
_diffrn_reflns_theta_full        68.391
_diffrn_reflns_theta_max         68.391
_diffrn_reflns_theta_min         3.623
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464.001
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.247
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.0351407
_refine_ls_shift/su_mean         0.0012279
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 3.29 4.21 1.23 0.160 0.743E-02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1711
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1711
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6178
_reflns_number_total             7199
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.33
_oxford_diffrn_Wilson_scale      81.95
_oxford_refine_ls_r_factor_ref   0.0728
_oxford_refine_ls_scale          0.12130(5)
_oxford_reflns_number_all        7199
_cod_data_source_file            d0cc05352j2.cif
_cod_data_source_block           7et_250K
_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 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C43 H53 N1 O6'
_cod_database_code               7127246
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)