Structural variety of heterosynthons in linezolid cocrystals with modified thermal properties
Khalaji, Mehrnaz; Wróblewska, Aneta; Wielgus, Ewelina; Bujacz, Grzegorz D.; Dudek, Marta K.; Potrzebowski, Marek J.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620010896

data_2108678
_publ_section_title
;
 Structural variety of heterosynthons in linezolid cocrystals with
 modified thermal properties
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620010896
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C16 H20 F N3 O4, C7 H6 O5, H2 O'
_chemical_formula_sum            'C23 H28 F N3 O10'
_chemical_formula_weight         525.48
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.7581(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.78184(17)
_cell_length_b                   15.47624(20)
_cell_length_c                   19.59820(18)
_cell_measurement_reflns_used    47167
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.3130
_cell_measurement_theta_min      2.6380
_cell_volume                     4898.74(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1685
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -125.00  -79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -99.0000   60.0000 46

  2 omega -125.00  -79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -99.0000  -60.0000 46

  3 omega -118.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -77.0000    0.0000 106

  4 omega  -49.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024   37.0000  -30.0000 77

  5 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  125.0000   90.0000 84

  6 omega   34.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -30.0000  150.0000 57

  7 omega   24.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -94.0000    0.0000 85

  8 omega   24.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -94.0000   60.0000 85

  9 omega   34.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -30.0000  120.0000 57

 10 omega   67.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   15.0000  -60.0000 111

 11 omega   36.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -45.0000   90.0000 62

 12 omega   34.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -30.0000  -60.0000 57

 13 omega -113.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -57.0000 -180.0000 95

 14 omega -113.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -57.0000   90.0000 95

 15 omega   23.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6024 -125.0000  150.0000 74

 16 omega   81.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   45.0000    0.0000 96

 17 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   30.0000 -180.0000 98

 18 omega   24.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -94.0000 -150.0000 85

 19 omega   36.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -45.0000   30.0000 62

 20 omega   75.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   77.0000   90.0000 103

 21 omega   81.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   45.0000   60.0000 96

 22 omega -118.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -77.0000   90.0000 106

 23 omega -125.00  -79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -99.0000 -150.0000 46

 24 omega -113.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.6024  -57.0000  -90.0000 95

 25 omega   36.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090  -45.0000 -150.0000 62

 26 omega   75.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   77.0000  -60.0000 103

 27 omega   75.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   77.0000    0.0000 103

 28 omega   75.00  166.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   77.0000  -90.0000 91

 29 omega   81.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7090   45.0000 -150.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0422110000
_diffrn_orient_matrix_UB_12      -0.0253587000
_diffrn_orient_matrix_UB_13      0.0773693000
_diffrn_orient_matrix_UB_21      -0.0815045000
_diffrn_orient_matrix_UB_22      0.0169041000
_diffrn_orient_matrix_UB_23      0.0196093000
_diffrn_orient_matrix_UB_31      -0.0259333000
_diffrn_orient_matrix_UB_32      -0.0947937000
_diffrn_orient_matrix_UB_33      -0.0172375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            79440
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.548
_diffrn_reflns_theta_min         2.342
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.4336
_exptl_crystal_size_mid          0.1779
_exptl_crystal_size_min          0.0714
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 7590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_coef       0.00065(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1366
_refine_ls_number_reflns         19039
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0790P)^2^+0.3717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.896
_reflns_Friedel_fraction_max     0.876
_reflns_number_gt                18059
_reflns_number_total             19039
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {8b9223d0-7960-4538-b2b8-30bbd45deed1}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            xk5072sup1.cif
_cod_data_source_block           LIN:GA:H2O
_cod_original_cell_volume        4898.74(9)
_cod_database_code               2108678
_cod_database_fobs_code          2108678
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C23H30F1N3O6
_reflns_odcompleteness_completeness 100.00
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
2.b Ternary CH refined with riding coordinates:
 C4A(H4A), C4B(H4B), C4C(H4C), C4D(H4D)
2.c Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C5A(H5AA,H5AB), C13A(H13A,H13B), C14A(H14A,H14B), C15A(H15A,
 H15B), C16A(H16A,H16B), C3B(H3BA,H3BB), C5B(H5BA,H5BB), C13B(H13C,H13D),
 C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D), C3C(H3CA,H3CB), C5C(H5CA,
 H5CB), C13C(H13E,H13F), C14C(H14E,H14F), C15C(H15E,H15F), C16D(H16E,H16F),
 C3D(H3DA,H3DB), C5D(H5DA,H5DB), C13D(H13G,H13H), C14D(H14G,H14H), C15D(H15G,
 H15H), C1(H1A,H1B)
2.d Aromatic/amide H refined with riding coordinates:
 N3A(H3A), C8A(H8A), C11A(H11A), C12A(H12A), N3B(H3B), C8B(H8B), C11B(H11B),
 C12B(H12B), N3C(H3C), C8C(H8C), C11C(H11C), C12C(H12C), N3D(H3D), C8D(H8D),
 C11D(H11D), C12D(H12D), C22A(H22A), C26A(H26A), C22B(H22B), C26B(H26B),
 C22C(H22C), C26C(H26C), C22D(H22D), C26D(H26D)
2.e Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC)
2.f Idealised tetrahedral OH refined as rotating group:
 O5A(H5A), O7A(H7A), O8A(H8AA), O9A(H9A), O5B(H5B), O7B(H7B), O8B(H8BA),
 O9B(H9B), O6C(H6C), O7C(H7C), O8C(H8CA), O9C(H9C), O6D(H6D), O7D(H7D),
 O8D(H8DA), O9D(H9D)
;
_shelx_res_checksum              1024
_shelx_hkl_checksum              39700
_olex2_date_sample_data_collection 2019-07-05
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;