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_4035810
_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 N8 Na, Br, 2(H2 O)'
_chemical_formula_sum            'C40 H52 Br N8 Na O2'
_chemical_formula_weight         779.79
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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                95.32(3)
_cell_angle_beta                 104.25(3)
_cell_angle_gamma                106.60(3)
_cell_formula_units_Z            3
_cell_length_a                   11.966(4)
_cell_length_b                   13.517(5)
_cell_length_c                   19.836(5)
_cell_measurement_reflns_used    2729
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.89
_cell_volume                     2933.8(18)
_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      103(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Kuma KM4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1309
_diffrn_reflns_av_unetI/netI     0.2105
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24498
_diffrn_reflns_point_group_measured_fraction_full 0.650
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.555
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.002(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1455
_refine_ls_number_reflns         14241
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1837
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2642
_reflns_Friedel_coverage         0.299
_reflns_Friedel_fraction_full    0.302
_reflns_Friedel_fraction_max     0.299
_reflns_number_gt                7128
_reflns_number_total             14241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00670_si_002.cif
_cod_data_source_block           '[Na+_R-6]Br.2H2O_(aku28ab)'
_cod_original_cell_volume        2933.8(17)
_cod_database_code               4035810
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.453
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              71751
_shelx_hkl_checksum              21407