A Magnetostructural Investigation of an Abrupt Spin Transition for 1-Phenyl-3-trifluoromethyl-1,4-dihydrobenzo[e][1,2,4]triazin-4-yl.
Constantinides, Christos P.; Berezin, Andrey A.; Zissimou, Georgia A.; Manoli, Maria; Leitus, Gregory M.; Bendikov, Michael; Probert, Michael R.; Rawson, Jeremy M.; Koutentis, Panayiotis A.; Journal of the American Chemical Society 136 (2014) 11906–; doi:10.1021/ja5063746

data_4122377
_publ_section_title
;
 A Magnetostructural Investigation of an Abrupt Spin Transition for
 1-Phenyl-3-trifluoromethyl-1,4-dihydrobenzo[e][1,2,4]triazin-4-yl.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11906
_journal_paper_doi               10.1021/ja5063746
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C14 H9 F3 N3'
_chemical_formula_sum            'C14 H9 F3 N3'
_chemical_formula_weight         276.24
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-01
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.19 svn.r2915 for OlexSys, GUI svn.r4811)
;
_cell_angle_alpha                79.778(2)
_cell_angle_beta                 67.137(2)
_cell_angle_gamma                86.490(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2531(4)
_cell_length_b                   8.6096(4)
_cell_length_c                   9.5178(4)
_cell_measurement_reflns_used    6863
_cell_measurement_temperature    75.0
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.36
_cell_volume                     613.25(5)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      75.0
_diffrn_detector                 'Bruker APEX-II CCD area detector'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.809
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measurement_device       'XIPHOS four-circle diffractometer'
_diffrn_measurement_device_type  Xiphos
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support '0.5mm graphite fibre'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.809
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9462
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.449
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'Bruker TXS with Helios Optics'
_diffrn_source_current           75.0
_diffrn_source_power             3.75
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8758.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       needle
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0224P)^2^+0.4491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1741
_reflns_number_total             2036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5063746_si_003.cif
_cod_data_source_block           data75k
_cod_depositor_comments
'Adding full bibliography for 4122377--4122379.cif.'
_cod_database_code               4122377
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              67556
_shelx_hkl_checksum              88087