A first-order phase transition in Blatter's radical at high pressure
Broadhurst, Edward T.; Wilson, Cameron J. G.; Zissimou, Georgia A.; Nudelman, Fabio; Constantinides, Christos P.; Koutentis, Panayiotis A.; Parsons, Simon; Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 78 (2022) –; doi:10.1107/S2052520622000191

data_2022560
_publ_section_title
;
 A first-order phase transition in Blatter's radical at high pressure
;
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_paper_doi               10.1107/S2052520622000191
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C19 H14 N3'
_chemical_formula_sum            'C19 H14 N3'
_chemical_formula_weight         284.33
_chemical_name_systematic        1,3-Diphenyl-1,2,4-benzotriazin-4(1H)-yl
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.934(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0953(4)
_cell_length_b                   6.1527(3)
_cell_length_c                   18.8502(18)
_cell_measurement_reflns_used    1769
_cell_measurement_temperature    270.8
_cell_measurement_theta_max      25.503
_cell_measurement_theta_min      3.489
_cell_volume                     1153.29(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      270.8
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.354
_diffrn_measured_fraction_theta_max 0.327
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.354
_diffrn_reflns_Laue_measured_fraction_max 0.327
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6509
_diffrn_reflns_point_group_measured_fraction_full 0.354
_diffrn_reflns_point_group_measured_fraction_max 0.327
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.345
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0612 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.9141.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_preparation       'As received'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.106
_refine_diff_density_min         -0.112
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         772
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0535P)^2^+0.2042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                518
_reflns_number_total             772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            um5054sup1.cif
_cod_data_source_block           sp20042_0m_4p0054GPa
_cod_database_code               2022560
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-N1
 1.361 with sigma of 0.01
 C3-N1
 1.401 with sigma of 0.01
 C3-N2
 2.417 with sigma of 0.03
 C14-N1
 1.427 with sigma of 0.01
 C14-N2
 2.342 with sigma of 0.03
 C14-C3
 2.488 with sigma of 0.03
 C1-N2
 1.336 with sigma of 0.01
 C1-N1
 2.289 with sigma of 0.03
 N3-C1
 1.325 with sigma of 0.01
 N3-N2
 2.388 with sigma of 0.03
 C8-C1
 1.489 with sigma of 0.01
 C8-N2
 2.375 with sigma of 0.03
 C8-N3
 2.413 with sigma of 0.03
 C2-N3
 1.375 with sigma of 0.01
 C2-C1
 2.287 with sigma of 0.03
 C7-C2
 1.392 with sigma of 0.01
 C7-N3
 2.395 with sigma of 0.03
 C3-C2
 1.408 with sigma of 0.01
 C3-N3
 2.434 with sigma of 0.03
 C3-C7
 2.401 with sigma of 0.03
 C6-C7
 1.372 with sigma of 0.01
 C6-C2
 2.411 with sigma of 0.03
 C5-C6
 1.389 with sigma of 0.01
 C5-C7
 2.386 with sigma of 0.03
 C4-C5
 1.375 with sigma of 0.01
 C4-C6
 2.404 with sigma of 0.03
 C3-C4
 1.39 with sigma of 0.01
 C3-C5
 2.388 with sigma of 0.03
 C19-C14
 1.374 with sigma of 0.01
 C19-N1
 2.43 with sigma of 0.03
 C15-C14
 1.374 with sigma of 0.01
 C15-N1
 2.415 with sigma of 0.03
 C15-C19
 2.385 with sigma of 0.03
 C18-C19
 1.384 with sigma of 0.01
 C18-C14
 2.381 with sigma of 0.03
 C17-C18
 1.356 with sigma of 0.01
 C17-C19
 2.382 with sigma of 0.03
 C16-C17
 1.374 with sigma of 0.01
 C16-C18
 2.361 with sigma of 0.03
 C15-C16
 1.387 with sigma of 0.01
 C15-C17
 2.396 with sigma of 0.03
 C9-C8
 1.393 with sigma of 0.01
 C9-C1
 2.488 with sigma of 0.03
 C13-C8
 1.379 with sigma of 0.01
 C13-C1
 2.511 with sigma of 0.03
 C13-C9
 2.384 with sigma of 0.03
 C10-C9
 1.383 with sigma of 0.01
 C10-C8
 2.403 with sigma of 0.03
 C11-C10
 1.362 with sigma of 0.01
 C11-C9
 2.388 with sigma of 0.03
 C12-C11
 1.373 with sigma of 0.01
 C12-C10
 2.365 with sigma of 0.03
 C13-C12
 1.379 with sigma of 0.01
 C13-C11
 2.387 with sigma of 0.03
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C19(H19), C18(H18), C17(H17), C16(H16),
 C15(H15), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              72516
_shelx_hkl_checksum              41318
_olex2_exptl_crystal_mounting_method 'Merrill Bassett diamond anvil cell'
_olex2_submission_original_sample_id SP20042
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2022560