Pasteur's tartaramide/malamide quasiracemates: new entries and departures from near inversion symmetry
Pinter, Emily N.; Cantrell, Lee S.; Day, Graeme M.; Wheeler, Kraig A.; CrystEngComm 20 (2018) 4213–; doi:10.1039/C8CE00791H

data_7230992
_publ_section_title
;
 Pasteur's tartaramide/malamide quasiracemates: new entries and departures
 from near inversion symmetry
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              4213
_journal_paper_doi               10.1039/C8CE00791H
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C12 H24 N2 O3, C12 H24 N2 O4'
_chemical_formula_sum            'C24 H48 N4 O7'
_chemical_formula_weight         504.66
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-24 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                102.543(7)
_cell_angle_beta                 96.249(5)
_cell_angle_gamma                90.472(5)
_cell_formula_units_Z            1
_cell_length_a                   4.9064(3)
_cell_length_b                   8.7118(6)
_cell_length_c                   17.1527(14)
_cell_measurement_reflns_used    6351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.056
_cell_measurement_theta_min      2.654
_cell_volume                     711.03(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.10-0 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15213
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.165
_diffrn_reflns_theta_min         2.656
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.5209
_exptl_absorpt_correction_T_min  0.4372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;   
 SADABS-2014/5 (Bruker,2014/5) was used for absorption
 correction. wR2(int) was 0.0725 before and 0.0530
 after correction. The Ratio of minimum to maximum
 transmission is 0.8393. The \l/2 correction
 factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.16(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4727
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0599P)^2^+0.2364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                4188
_reflns_number_total             4727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00791h2.cif
_cod_data_source_block           kaw13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7230989--7230996.cif.
;
_cod_database_code               7230992
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              88077