Chiral Cryptates Derived from a Hexaazamacrocycle.
Gerus, Aleksandra; Ślepokura, Katarzyna; Panek, Jarosław; Turek, Aleksandra; Lisowski, Jerzy; The Journal of organic chemistry 83 (2018) 6748–6753; doi:10.1021/acs.joc.8b00670

data_4035811
_publ_section_title
;
 Chiral Cryptates Derived from a Hexaazamacrocycle.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6748
_journal_page_last               6753
_journal_paper_doi               10.1021/acs.joc.8b00670
_journal_volume                  83
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C40 H48 K N8, Br, 0.7(C H4 O), 0.9(H2 O)'
_chemical_formula_sum            'C40.7 H52.6 Br K N8 O1.6'
_chemical_formula_weight         798.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.30(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.092(4)
_cell_length_b                   27.403(8)
_cell_length_c                   23.358(9)
_cell_measurement_reflns_used    4941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.72
_cell_volume                     7727(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Technologies, Xcalibur R, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31263
_diffrn_reflns_point_group_measured_fraction_full 0.749
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             3357
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 3059 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1905
_refine_ls_number_reflns         20409
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.467
_reflns_Friedel_fraction_full    0.488
_reflns_Friedel_fraction_max     0.488
_reflns_number_gt                12798
_reflns_number_total             20409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00670_si_002.cif
_cod_data_source_block           '[K+_R-6]Br.7/10MeOH.9/10H2O_(aku22)'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C40.70 H52.60 Br K N8 O1.60'
_cod_database_code               4035811
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              169
_shelx_hkl_checksum              95644