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_2108675
_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_formula_moiety         'C16 H20 F N3 O4, C7 H6 O3, H2 O'
_chemical_formula_sum            'C23 H28 F N3 O8'
_chemical_formula_weight         492.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.428(3)
_cell_length_b                   6.987(3)
_cell_length_c                   52.001(9)
_cell_measurement_reflns_used    4747
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      3.3110
_cell_volume                     2335.5(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3370
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -115.00  -5.00   1.00   20.00    --  -37.73 -19.00 150.00  110
  2  \w    -49.00  34.00   1.00   20.00    --  -37.73  37.00-150.00   83
  3  \w     55.00 125.00   1.00   20.00    --   37.73-178.00-120.00   70
  4  \w     37.00  98.00   1.00   60.00    --  108.00 -45.00  30.00   61
  5  \w     37.00  98.00   1.00   60.00    --  108.00 -45.00-150.00   61
  6  \w     84.00 178.00   1.00   60.00    --  108.00  45.00 120.00   94
  7  \w     35.00  91.00   1.00   60.00    --  108.00 -30.00 150.00   56
  8  \w     94.00 178.00   1.00   60.00    --  108.00 125.00 -60.00   84
  9  \w   -107.00 -12.00   1.00   20.00    --  -37.73 -57.00  60.00   95
 10  \w   -107.00 -12.00   1.00   20.00    --  -37.73 -57.00 -60.00   95
 11  \w     81.00 178.00   1.00   60.00    --  108.00  61.00-180.00   97
 12  \w     25.00 109.00   1.00   60.00    --  108.00 -94.00   0.00   84
 13  \w     69.00 178.00   1.00   60.00    --  108.00  15.00  60.00  109
 14  \w     69.00 178.00   1.00   60.00    --  108.00  15.00 -60.00  109
 15  \w    -49.00  34.00   1.00   20.00    --  -37.73  37.00 -60.00   83
 16  \w     57.00 127.00   1.00   20.00    --   37.73 178.00  90.00   70
 17  \w     25.00 109.00   1.00   60.00    --  108.00 -94.00-120.00   84
 18  \w     81.00 178.00   1.00   60.00    --  108.00  61.00-150.00   97
 19  \w     81.00 146.00   1.00   60.00    --  108.00  61.00 150.00   65
 20  \w     84.00 178.00   1.00   60.00    --  108.00  45.00 -30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2100813000
_diffrn_orient_matrix_UB_12      -0.0970546000
_diffrn_orient_matrix_UB_13      -0.0056962000
_diffrn_orient_matrix_UB_21      0.0438058000
_diffrn_orient_matrix_UB_22      -0.1489472000
_diffrn_orient_matrix_UB_23      0.0211570000
_diffrn_orient_matrix_UB_31      -0.1067498000
_diffrn_orient_matrix_UB_32      0.1304043000
_diffrn_orient_matrix_UB_33      0.0199399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.187
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            8325
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.485
_diffrn_reflns_theta_max         67.485
_diffrn_reflns_theta_min         3.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       needle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.280
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   1.5(6)
_refine_ls_extinction_coef       0.031(10)
_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   1.652
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         8325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.652
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3683
_refine_ls_wR_factor_ref         0.3967
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.819
_reflns_Friedel_fraction_max     0.819
_reflns_number_gt                6511
_reflns_number_total             8325
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9016\% 
 around [-0.00 0.00 1.00] (reciprocal) or [-0.02 0.03 1.00] (direct)
Component 3 rotated by -179.8894\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [-0.03 -0.09 1.00] (direct)
Component 4 rotated by 1.6244\% 
 around [-0.84 0.12 0.53] (reciprocal) or [-0.99 0.12 0.01] (direct)
;
_publcif_datablock.id            {6a42a544-6e46-4555-ab69-39fabfdf7f9d}
_cod_data_source_file            xk5072sup1.cif
_cod_data_source_block           LIN:PHBA:H2O
_cod_database_code               2108675
_cod_database_fobs_code          2108675
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.23(5)
 0.23(5) 0.338(7) 0.197(6)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C8)
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C4(H4)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B)
4.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C8(H8), C11(H11), C12(H12), C22(H22), C23(H23), C25(H25), C26(H26)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
4.f Idealised tetrahedral OH refined as rotating group:
 O6(H6), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.617
_oxdiff_exptl_absorpt_empirical_full_min 0.281
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4