Dual-rotor strategy for organic cocrystals with enhanced near-infrared photothermal conversion
Wen, Xinyi; Shao, Yixin; Chen, Ye-Tao; He, Jiaxing; Chen, Shun-Li; Dang, Li; Li, Ming-De; RSC Advances 14 (2024) 4503–4508; doi:10.1039/D4RA00002A

data_7248092
_publ_section_title
;
 Dual-rotor strategy for organic cocrystals with enhanced near-infrared
 photothermal conversion
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              4503
_journal_page_last               4508
_journal_paper_doi               10.1039/D4RA00002A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         '2(C6 F2 N2), 2(C8 H7)'
_chemical_formula_sum            'C28 H14 F4 N4'
_chemical_formula_weight         482.43
_chemical_name_systematic        DFQ
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-04
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-04 deposited with the CCDC.	2024-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                82.874(2)
_cell_angle_beta                 80.374(2)
_cell_angle_gamma                83.233(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7988(2)
_cell_length_b                   8.4619(2)
_cell_length_c                   16.7251(4)
_cell_measurement_reflns_used    7719
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      70.7740
_cell_measurement_theta_min      2.6690
_cell_volume                     1074.46(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.960
_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     56.00  89.00   0.50    0.50    --    0.00  57.00-180.00   66
  2  \w    -25.00   6.00   0.50    0.50    --    0.00  82.00   0.00   62
  3  \w    -19.00   8.00   0.50    0.50    --    0.00  37.00  90.00   54
  4  \w    -18.00  18.00   0.50    0.50    --    0.00  57.00-180.00   72
  5  \w     35.00  84.00   0.50    0.50    --    0.00  82.00   0.00   98
  6  \w     59.00  89.00   0.50    0.50    --    0.00  37.00  90.00   60
  7  \w    131.00 173.00   0.50    1.42    --   89.30  45.00 150.00   84
  8  \w     85.00 125.00   0.50    1.42    --   89.30  45.00 150.00   80
  9  \w      0.00  71.00   0.50    1.42    --   89.30 -15.00-180.00  142
 10  \w      1.00 118.00   0.50    1.42    --   89.30 -82.00 150.00  234
 11  \w      0.00  42.00   0.50    1.42    --   89.30 -61.00 -90.00   84
 12  \w     47.00 114.00   0.50    1.42    --   89.30 -61.00 -90.00  134
 13  \w     77.00 103.00   0.50    1.42    --   89.30 -82.00  90.00   52
 14  \w      1.00 102.00   0.50    1.42    --   89.30 -61.00 150.00  202
 15  \w     31.00  66.00   0.50    1.42    --   89.30 -82.00  90.00   70
 16  \w     25.00 113.00   0.50    1.42    --   89.30 -15.00 -30.00  176
 17  \w     21.00 118.00   0.50    1.42    --   89.30 -82.00 -90.00  194
 18  \w     48.00  74.00   0.50    1.42    --   89.30 -77.00  30.00   52
 19  \w     91.00 116.00   0.50    1.42    --   89.30 -77.00  30.00   50
 20  \w      2.00  28.00   0.50    1.42    --   89.30 -82.00   0.00   52
 21  \w     37.00 120.00   0.50    1.42    --   89.30 -82.00   0.00  166
 22  \w    121.00 146.00   0.50    1.42    --   89.30  30.00-180.00   50
 23  \w     78.00 103.00   0.50    1.42    --   89.30 -82.00  30.00   50
 24  \w     77.00 117.00   0.50    1.42    --   89.30 -15.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035814000
_diffrn_orient_matrix_UB_12      -0.1693638000
_diffrn_orient_matrix_UB_13      0.0461283000
_diffrn_orient_matrix_UB_21      0.0591598000
_diffrn_orient_matrix_UB_22      -0.0726244000
_diffrn_orient_matrix_UB_23      -0.0813701000
_diffrn_orient_matrix_UB_31      0.1924321000
_diffrn_orient_matrix_UB_32      0.0063320000
_diffrn_orient_matrix_UB_33      0.0089317000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10185
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.000
_diffrn_reflns_theta_min         2.695
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0557P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3781
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra00002a2.cif
_cod_data_source_block           20211030c
_cod_database_code               7248092
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F'
_chemical_oxdiff_usercomment     'C H N F'
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00P(H00P), C00R(H00R), C00T(H00T), C00V(H00V), C00W(H00W),
 C00Z(H00Z), C010(H010)
2.b Idealised Me refined as rotating group:
 C00N(H00D,H00E,H00F), C00Y(H00A,H00B,H00C)
;
_shelx_res_checksum              32138
_shelx_hkl_checksum              20354
_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 1.327
_oxdiff_exptl_absorpt_empirical_full_min 0.644