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_7248090
_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         'C12 H4 N4, C15 H12'
_chemical_formula_sum            'C27 H16 N4'
_chemical_formula_weight         396.44
_chemical_name_systematic        MTQ
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 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                90
_cell_angle_beta                 98.472(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1900(5)
_cell_length_b                   13.4371(5)
_cell_length_c                   7.0568(3)
_cell_measurement_reflns_used    1065
_cell_measurement_temperature    299.82(10)
_cell_measurement_theta_max      67.4810
_cell_measurement_theta_min      5.1830
_cell_volume                     1049.49(8)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.82(10)
_diffrn_detector                 'CCD plate'
_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    -19.00   8.00   0.50    1.00    --    0.00 -37.00 -60.00   54
  2  \w    -89.00 -34.00   0.50    1.00    --    0.00 -37.00 -60.00  110
  3  \w    -17.00  17.00   0.50    1.00    --    0.00  37.00-180.00   68
  4  \w     54.00  80.00   0.50    1.00    --    0.00  37.00-180.00   52
  5  \w     79.00 134.00   0.50    4.01    --   89.30  61.00 120.00  110
  6  \w      3.00 108.00   0.50    4.01    --   89.30 -82.00-180.00  210
  7  \w     50.00 103.00   0.50    4.01    --   89.30 -61.00  30.00  106
  8  \w    140.00 177.00   0.50    4.01    --   89.30  61.00 120.00   74
  9  \w      6.00 119.00   0.50    4.01    --   89.30 -77.00 -30.00  226
 10  \w     82.00 118.00   0.50    4.01    --   89.30  30.00-180.00   72
 11  \w     97.00 158.00   0.50    4.01    --   89.30  45.00  30.00  122
;
_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      -0.0662679000
_diffrn_orient_matrix_UB_12      0.0987059000
_diffrn_orient_matrix_UB_13      -0.0544271000
_diffrn_orient_matrix_UB_21      0.1222603000
_diffrn_orient_matrix_UB_22      0.0523938000
_diffrn_orient_matrix_UB_23      -0.0011183000
_diffrn_orient_matrix_UB_31      -0.0049967000
_diffrn_orient_matrix_UB_32      -0.0253071000
_diffrn_orient_matrix_UB_33      -0.2141145000
_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  0.0153
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2115
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        59.971
_diffrn_reflns_theta_max         59.971
_diffrn_reflns_theta_min         5.177
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54752
_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            green
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       0.0023(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         813
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.398
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0994P)^2^+0.5098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                673
_reflns_number_total             813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra00002a2.cif
_cod_data_source_block           20220303d
_cod_database_code               7248090
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N'
_chemical_oxdiff_usercomment     'C H N'
_reflns_odcompleteness_completeness 99.47
_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. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C6 \\sim C4: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: H4(0.25) C18(0.25) H18a(0.25) H18b(0.25) H18c(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C4(H4), C13(H13), C14(H14)
4.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c)
;
_shelx_res_checksum              32164
_shelx_hkl_checksum              85266
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.821