Non-equimolar discrete compounds in binary chiral systems of organic substances
Kotelnikova, Elena N.; Isakov, Anton I.; Lorenz, Heike; CrystEngComm 19 (2017) 1851–; doi:10.1039/C6CE02209J

data_7227923
_publ_section_title
;
 Non-equimolar discrete compounds in binary chiral systems of organic
 substances
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              1851
_journal_paper_doi               10.1039/C6CE02209J
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C5.48 H11.66 N O2, C5.37 H10.92 N O2'
_chemical_formula_sum            'C10.85 H22.57 N2 O4'
_chemical_formula_weight         245.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1l9k3k
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.215(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7697(14)
_cell_length_b                   5.2445(2)
_cell_length_c                   9.6681(6)
_cell_measurement_reflns_used    2138
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.2070
_cell_measurement_theta_min      4.5940
_cell_volume                     1296.29(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354   38.0000   30.0000 82

  2 omega  -64.00  -37.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354  178.0000  -60.0000 27

  3 omega  -83.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354  178.0000    0.0000 48

  4 omega -114.00  -13.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354  -57.0000 -120.0000 101

  5 omega   34.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -30.0000 -120.0000 56

  6 omega   96.00  138.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -61.0000  -90.0000 42

  7 omega  104.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -61.0000 -120.0000 26

  8 omega  105.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -15.0000    0.0000 47

  9 omega   85.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760   30.0000   30.0000 93

 10 omega   88.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760 -125.0000   90.0000 31

 11 omega   52.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -95.0000  -30.0000 57

 12 omega   60.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -61.0000 -120.0000 26

 13 omega   40.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -45.0000 -150.0000 41

 14 omega   39.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760 -125.0000  -90.0000 80

 15 omega   40.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -77.0000   60.0000 101

 16 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760 -125.0000   90.0000 27

 17 omega   37.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -30.0000  120.0000 40

 18 omega   44.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3760  -30.0000   60.0000 13
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0573452000
_diffrn_orient_matrix_UB_12      0.0884447000
_diffrn_orient_matrix_UB_13      -0.0110314000
_diffrn_orient_matrix_UB_21      0.0003433000
_diffrn_orient_matrix_UB_22      0.0536077000
_diffrn_orient_matrix_UB_23      -0.1565250000
_diffrn_orient_matrix_UB_31      -0.0184875000
_diffrn_orient_matrix_UB_32      -0.2749317000
_diffrn_orient_matrix_UB_33      -0.0343624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3474
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.951
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       prism
_exptl_crystal_F_000             535
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1590
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0962P)^2^+0.0203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                1531
_reflns_number_total             1590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02209j2.cif
_cod_data_source_block           V2I
_cod_depositor_comments
'Adding full bibliography for 7227922--7227923.cif.'
_cod_database_code               7227923
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C10 H10 O5 N5'
_reflns_odcompleteness_completeness 95.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8D,H8E), C9(H9A,H9B)
2.c Idealised Me refined as rotating group:
 N7(H7D,H7E,H7F), N8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              57734
_olex2_submission_special_instructions 'No special instructions were received'