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_7230116
_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, 2(C6 H10 O)'
_chemical_formula_sum            'C38 H50 N8 O6'
_chemical_formula_weight         714.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-05
_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                90
_cell_angle_beta                 92.145(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.641(3)
_cell_length_b                   16.911(3)
_cell_length_c                   26.532(4)
_cell_measurement_reflns_used    3019
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      22.34
_cell_measurement_theta_min      2.27
_cell_volume                     7461(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1666
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12006
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.928
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.1453 before and 0.1220 after correction.
 The Ratio of minimum to maximum transmission is 0.63.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 60605 reflections, Rint = 0.2063
 (14706 with I > 3sig(I), Rint = 0.1263)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         12006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.1197
_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^)+(0.0900P)^2^+13.5850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7681
_reflns_number_total             12006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00066b2.cif
_cod_data_source_block           2Cycl_twin
_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 7230114--7230119.cif.
;
_cod_database_code               7230116
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.974
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.531(2)
 0.469(2)
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
3.a Riding coordinates:
 N6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,
 H6SB), C2SA(H2SC,H2SD), C3SA(H3SC,H3SD), C4SA(H4SC,H4SD), C5SA(H5SC,H5SD),
 C6SA(H6SC,H6SD), C2SB(H2SE,H2SF), C3SB(H3SE,H3SF), C4SB(H4SE,H4SF), C5SB(H5SE,
 H5SF), C6SB(H6SE,H6SF), C2SC(H2SG,H2SH), C3SC(H3SG,H3SH), C4SC(H4SG,H4SH),
 C5SC(H5SG,H5SH), C6SC(H6SG,H6SH)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N5(H5), N7(H7), C1(H1), C2(H2A), C4(H4A), C5(H5A),
 C12(H12), C13(H13), C14(H14), C16(H16), C23(H23), C24(H24), C25(H25), C26(H26),
  N2A(H2AA), N3A(H3A), N4A(H4AA), N5A(H5AA), N6A(H6A), N7A(H7A), C1A(H1A),
 C2A(H2AB), C4A(H4AB), C5A(H5AB), C12A(H12A), C13A(H13A), C14A(H14A),
 C16A(H16A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A)
3.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)
;
_olex2_submission_special_instructions 'No special instructions were received'