Bowl-shaped Tröger's bases and their recognition properties.
Mosca, Lorenzo; Čejka, Jan; Dolenský, Bohumil; Havlík, Martin; Jakubek, Milan; Kaplánek, Robert; Král, Vladimír; Anzenbacher, Pavel; Chemical communications (Cambridge, England) 52 (2016) 10664–10667; doi:10.1039/c6cc05923f

data_7124968
_publ_section_title
;
 Bowl-shaped Tr\"oger's bases and their recognition properties.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10664
_journal_page_last               10667
_journal_paper_doi               10.1039/c6cc05923f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C51 H41.00 N7 O2'
_chemical_formula_sum            'C51 H41 N7 O2'
_chemical_formula_weight         783.93
_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     direct
_audit_update_record
;
2016-06-13 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.101(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.998(6)
_cell_length_b                   14.423(6)
_cell_length_c                   21.871(9)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    180
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3782(3)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            54809
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.864
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1647.990
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.56
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0686
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6925
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.1093
_refine_ls_shift/su_max          0.0001101
_refine_ls_shift/su_mean         0.0000156
_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: 
 8.86 11.7 3.51 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3448
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.3448
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                4025
_reflns_number_total             6930
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.74
_oxford_diffrn_Wilson_scale      86.88
_oxford_refine_ls_r_factor_ref   0.1721
_oxford_refine_ls_scale          0.11894(12)
_oxford_reflns_number_all        6925
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S  U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) H   ( 852,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  N(1) C(4) C(5) C(6) C(7) C(8) C(9) 
DELU 0.010000  N(1) C(4) C(5) C(6) C(7) C(8) C(9) 
SIMU 0.010000  N(1) C(4) C(5) C(6) C(7) C(8) C(9) 
DISTANCE 1.420000 , 0.020000 = C(8) TO C(9) 
DISTANCE 1.420000 , 0.010000 = C(6) TO C(7) 
DISTANCE 1.420000 , 0.020000 = C(5) TO C(6) 
END                                                                             
;
_cod_data_source_file            c6cc05923f2.cif
_cod_data_source_block           calix-1_C6H5NO2
_cod_original_cell_volume        3782.1(15)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C51 H41.00 N7 O2'
_cod_database_code               7124968