Accessing Centnerszwer's quasiracemate – molecular shape controlled molecular recognition
Spaniol, Jacqueline M.; Wheeler, Kraig A.; RSC Adv. 6 (2016) 64921–; doi:10.1039/C6RA08131B

data_7225891
_publ_section_title
;
 Accessing Centnerszwer's quasiracemate -- molecular shape controlled
 molecular recognition
;
_journal_issue                   69
_journal_name_full               'RSC Adv.'
_journal_page_first              64921
_journal_paper_doi               10.1039/C6RA08131B
_journal_volume                  6
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '2(C10 H8 N2 O2), C4 H5 Br O4, C4 H5'
_chemical_formula_sum            'C28 H26 Br Cl N4 O12'
_chemical_formula_weight         725.89
_chemical_melting_point          457.0(10)
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-25 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                102.275(3)
_cell_angle_beta                 93.038(2)
_cell_angle_gamma                107.620(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7692(3)
_cell_length_b                   9.6937(5)
_cell_length_c                   10.7311(4)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.06
_cell_measurement_theta_min      4.25
_cell_volume                     746.66(6)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16717
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.223
_diffrn_reflns_theta_min         4.250
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/7, Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             370
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 1797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.0865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.764
_reflns_Friedel_fraction_max     0.759
_reflns_number_gt                4597
_reflns_number_total             4755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra08131b2.cif
_cod_data_source_block           15kaw14a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '456-458' was changed to '457.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7225891
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.626
_shelx_estimated_absorpt_t_max   0.878
_shelx_res_checksum              98830
_solvent_exptl_crystal_recrystallization_method methanol