Regioselective formation of the quinazoline moiety on the upper rim of calix[4]arene as a route to inherently chiral systems
Tlustý, M.; Dvořáková, H.; Čejka, J.; Kohout, M.; Lhoták, P.; New Journal of Chemistry 44 (2020) 6490–6500; doi:10.1039/D0NJ01035A

data_7059454
_publ_section_title
;
 Regioselective formation of the quinazoline moiety on the upper rim of
 calix[4]arene as a route to inherently chiral systems
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6490
_journal_page_last               6500
_journal_paper_doi               10.1039/D0NJ01035A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C54.50 H58 N2 O4.50'
_chemical_formula_sum            'C54.5 H58 N2 O4.5'
_chemical_formula_weight         813.07
_chemical_melting_point          405.5(15)
_chemical_name_systematic
'2,4-Diphenylquinazoline calixarene derivative'
_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_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2020-02-24 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7686(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5527(2)
_cell_length_b                   17.1196(4)
_cell_length_c                   28.2418(6)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    180
_cell_measurement_theta_max      48
_cell_measurement_theta_min      11
_cell_volume                     4616.42(17)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.030
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70675
_diffrn_reflns_theta_full        72.901
_diffrn_reflns_theta_max         74.389
_diffrn_reflns_theta_min         3.019
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.37
_refine_ls_extinction_coef       90(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.0008264
_refine_ls_shift/su_mean         0.0000993
_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: 
 18.5 30.3 17.0 6.25 1.12 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1564
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1564
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                8178
_reflns_number_total             9364
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.49
_oxford_diffrn_Wilson_scale      76.86
_oxford_refine_ls_r_factor_ref   0.0652
_oxford_refine_ls_scale          0.11765(6)
_oxford_reflns_number_all        9364
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            d0nj01035a2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '404-407' was changed to
'405.5(15)' -- the average value was taken and precision was
estimated.

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

 Adding full bibliography for 7059454.cif.

 Adding full bibliography for 7059454.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C54.50 H58 N2 O4.50'
_cod_database_code               7059454