Chiral Crystals from Dynamic Combinatorial Libraries of Achiral Macrocyclic Imines
Ziach, Krzysztof; Jurczak, Janusz; Crystal Growth & Design 15 (2015) 4372–; doi:10.1021/acs.cgd.5b00658

data_4513483
_publ_section_title
;
 Chiral Crystals from Dynamic Combinatorial Libraries of Achiral
 Macrocyclic Imines
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4372
_journal_paper_doi               10.1021/acs.cgd.5b00658
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C17 H20 Br N2 Na O3'
_chemical_formula_weight         403.25
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 102.9580(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9345(5)
_cell_length_b                   11.4411(6)
_cell_length_c                   8.9682(5)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.7865
_cell_measurement_theta_min      2.3304
_cell_volume                     893.39(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 V2013 (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Diamond 3.2 (Brandenburg & Putz, 2012)'
_computing_publication_material  'APEX2 V2013 (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  TRIUMPH
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14082
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.151
_refine_ls_abs_structure_details
;
Flack x determined using 1743 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0165(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0151
_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^)+(0.0147P)^2^+0.2042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                3740
_reflns_number_total             3807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00658_si_004.cif
_cod_data_source_block           1_NaBr_A
_cod_depositor_comments
'Adding full bibliography for 4513482--4513486.cif.'
_cod_database_code               4513483