Proflavine and zinc chloride “team chemistry”: combining antibacterial agents via solid-state interaction
Fiore, Cecilia; Shemchuk, Oleksii; Grepioni, Fabrizia; Turner, Raymond J.; Braga, Dario; CrystEngComm 23 (2021) 4494–4499; doi:10.1039/D1CE00612F

data_7242891
_publ_section_title
;
 Proflavine and zinc chloride &#x201C;team chemistry&#x201D;: combining
 antibacterial agents via solid-state interaction
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              4494
_journal_page_last               4499
_journal_paper_doi               10.1039/D1CE00612F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'Cl, 2(H2 O), C13 H12 N3'
_chemical_formula_sum            'C13 H16 Cl N3 O2'
_chemical_formula_weight         281.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-03 deposited with the CCDC.	2021-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.941(6)
_cell_angle_beta                 77.478(5)
_cell_angle_gamma                75.976(6)
_cell_formula_units_Z            4
_cell_length_a                   7.5170(5)
_cell_length_b                   12.5737(10)
_cell_length_c                   15.5867(10)
_cell_measurement_reflns_used    1644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.6030
_cell_measurement_theta_min      3.4310
_cell_volume                     1393.23(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -84.00   6.00   1.00  255.00    --  -16.28 -38.00  60.00   90
  2  \w    -39.00  36.00   1.00  255.00    --  -16.28  38.00 -90.00   75
  3  \w      6.00  52.00   1.00  255.00    --  -16.28  57.00   0.00   46
  4  \w    -85.00 -54.00   1.00  255.00    --  -16.28 -57.00-150.00   31
  5  \w    -16.00  58.00   1.00  255.00    --   17.77 -99.00 -30.00   74
  6  \w    -11.00  34.00   1.00  255.00    --   17.77  77.00  90.00   45
  7  \w     -3.00  22.00   1.00  255.00    --   17.77  77.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139598000
_diffrn_orient_matrix_UB_12      0.0578761000
_diffrn_orient_matrix_UB_13      0.0017086000
_diffrn_orient_matrix_UB_21      -0.0340587000
_diffrn_orient_matrix_UB_22      0.0018598000
_diffrn_orient_matrix_UB_23      0.0462614000
_diffrn_orient_matrix_UB_31      0.0927374000
_diffrn_orient_matrix_UB_32      -0.0061423000
_diffrn_orient_matrix_UB_33      0.0060353000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.237
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2209
_reflns_number_total             4882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00612f2.cif
_cod_data_source_block           pf_zncl2_batch2-1_test_r1
_cod_depositor_comments
'Adding full bibliography for 7242890--7242893.cif.'
_cod_database_code               7242891
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O003(H00J,H00K), O005(H00O,H00Q), O007(H00R,H00T), O008(H00X,H00)
2.b Rotating group:
 N009(H00E,H00G), N00B(H00C,H00D)
2.c Aromatic/amide H refined with riding coordinates:
 N004(H004), N006(H006), C00F(H00F), C00L(H00L), C00M(H00M), C00N(H00N),
 C00P(H00P), C00S(H00S), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C012(H012)
2.d X=CH2 refined with riding coordinates:
 N00A(H00A,H00B), N00J(H00H,H00I)
;
_shelx_res_checksum              85608
_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 1.073
_oxdiff_exptl_absorpt_empirical_full_min 0.934