Polymorphism in a π Stacked Blatter Radical: Structures and Magnetic Properties of 3-(Phenyl)-1-(pyrid-2-yl)-1,4-dihydrobenzo[e][1,2,4]triazin-4-yl
Constantinides, Christos P.; Lawson, Daniel B.; Zissimou, Georgia; Berezin, Andrey; Mailman, Aaron M.; Manoli, Maria; Kourtellaris, Andreas; Leitus, Gregory; Clerac, Rodolphe; Tuononen, Heikki M.; Koutentis, Panayiotis Andreas; CrystEngComm  (2020) –; doi:10.1039/D0CE00789G

data_7240968
_publ_section_title
;
 Polymorphism in a \p Stacked Blatter Radical: Structures and Magnetic
 Properties of
 3-(Phenyl)-1-(pyrid-2-yl)-1,4-dihydrobenzo[e][1,2,4]triazin-4-yl
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00789G
_journal_year                    2020
_chemical_formula_moiety         'C18 H13 N4'
_chemical_formula_sum            'C18 H13 N4'
_chemical_formula_weight         285.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-16 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1656(3)
_cell_length_b                   10.9705(4)
_cell_length_c                   17.5843(6)
_cell_measurement_reflns_used    2053
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.8390
_cell_measurement_theta_min      4.7030
_cell_volume                     1382.31(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -63.00  19.00   1.00    1.50    --  -42.15  57.00  90.00   82
  2  \w      1.00  34.00   1.00    1.50    --   42.15 -99.00   0.00   33
  3  \w     30.00  88.00   1.00    1.50    --   42.15-125.00 -90.00   58
  4  \w     54.00  80.00   1.00    6.00    --  112.00-111.00 150.00   26
  5  \w    130.00 178.00   1.00    6.00    --  112.00 111.00   0.00   48
  6  \w    100.00 144.00   1.00    6.00    --  112.00 111.00-120.00   44
  7  \w     85.00 120.00   1.00    6.00    --  112.00  30.00-150.00   35
  8  \w    101.00 155.00   1.00    6.00    --  112.00 111.00 -90.00   54
  9  \w    141.00 167.00   1.00    6.00    --  112.00  30.00-150.00   26
 10  \w     37.00  62.00   1.00    6.00    --  112.00-111.00 -60.00   25
 11  \w    132.00 165.00   1.00    6.00    --  112.00  30.00 150.00   33
 12  \w     86.00 178.00   1.00    6.00    --  112.00  45.00  30.00   92
 13  \w    116.00 164.00   1.00    6.00    --  112.00 111.00-150.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0608074000
_diffrn_orient_matrix_UB_12      -0.0208612000
_diffrn_orient_matrix_UB_13      -0.0830139000
_diffrn_orient_matrix_UB_21      -0.1390887000
_diffrn_orient_matrix_UB_22      -0.1065810000
_diffrn_orient_matrix_UB_23      -0.0065865000
_diffrn_orient_matrix_UB_31      -0.1522149000
_diffrn_orient_matrix_UB_32      0.0891490000
_diffrn_orient_matrix_UB_33      -0.0270889000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5012
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.490
_diffrn_reflns_theta_min         4.751
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             596
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 846 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0559P)^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         0.1001
_reflns_Friedel_coverage         0.629
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.874
_reflns_number_gt                2374
_reflns_number_total             2674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00789g2.cif
_cod_data_source_block           alpha-phase-ortho
_cod_database_code               7240968
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H13 N4'
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18)
;
_ins_header
;
TITL alpha-phase-ortho in P2(1)2(1)2(1) 
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184   7.165591  10.970526  17.584296  90.0000  90.0000  90.0000
ZERR    4.00   0.000252   0.000444   0.000636   0.0000   0.0000   0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N
UNIT 72.00 52.00 16.00
TREF
HKLF 4
END
;
_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 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.768