Tailored supramolecular gel and microemulsion crystallization strategies – is isoniazid really monomorphic?
Kennedy, Stuart R.; Jones, Christopher D.; Yufit, Dmitry S.; Nicholson, Catherine E.; Cooper, Sharon J.; Steed, Jonathan W.; CrystEngComm 20 (2018) 1390–; doi:10.1039/C8CE00066B

data_7230119
_publ_section_title
;
 Tailored supramolecular gel and microemulsion crystallization strategies
 -- is isoniazid really monomorphic?
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1390
_journal_paper_doi               10.1039/C8CE00066B
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C26 H30 N8 O4, C7 H9 N'
_chemical_formula_sum            'C33 H39 N9 O4'
_chemical_formula_weight         625.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-15 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                84.489(4)
_cell_angle_beta                 67.608(5)
_cell_angle_gamma                82.921(4)
_cell_formula_units_Z            4
_cell_length_a                   13.3968(8)
_cell_length_b                   16.0797(6)
_cell_length_c                   16.7219(8)
_cell_measurement_reflns_used    13063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4530
_cell_measurement_theta_min      1.6090
_cell_volume                     3300.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Synchrotron '
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37133
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.827
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plank
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         17743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0960P)^2^+0.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12650
_reflns_number_total             17743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00066b2.cif
_cod_data_source_block           2etpyd
_cod_depositor_comments
'Adding full bibliography for 7230114--7230119.cif.'
_cod_original_cell_volume        3300.5(3)
_cod_database_code               7230119
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.988
_oxdiff_exptl_absorpt_empirical_full_min 0.301
_oxdiff_exptl_absorpt_empirical_full_max 4.691
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_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
2.a Riding coordinates:
 N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N2A(H2AA), N3A(H3A),
 N4A(H4AA), N5A(H5AA), N6A(H6A), N7A(H7A)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C4(H4A), C5(H5A), C12(H12), C13(H13), C14(H14), C16(H16),
 C23(H23), C24(H24), C25(H25), C26(H26), C1A(H1A), C2A(H2AB), C4A(H4AB),
 C5A(H5AB), C12A(H12A), C13A(H13A), C14A(H14A), C16A(H16A), C23A(H23A),
 C24A(H24A), C25A(H25A), C26A(H26A), C27(H27), C28(H28), C30(H30), C31(H31),
 C34(H34), C35(H35), C37(H37), C38(H38)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'