Probing through-space and through-bond magnetic exchange couplings in a new benzotriazinyl radical and its metal complexes.
Nasani, Rajendar; Sidharth, Thulaseedharan Nair Sailaja; Roy, Subhadip; Mondal, Arpan; Rawson, Jeremy M.; Konar, Sanjit; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14189–14200; doi:10.1039/c9dt01918a

data_7700881
_publ_section_title
;
 Probing through-space and through-bond magnetic exchange couplings in a
 new benzotriazinyl radical and its metal complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14189
_journal_page_last               14200
_journal_paper_doi               10.1039/c9dt01918a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C29 H14 F15 N4 Ni O4'
_chemical_formula_sum            'C29 H14 F15 N4 Ni O4'
_chemical_formula_weight         826.15
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-26
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2018-12-02 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.376(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6466(19)
_cell_length_b                   23.027(4)
_cell_length_c                   21.015(3)
_cell_measurement_reflns_used    51789
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.30
_cell_volume                     6367.4(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.239
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/2
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       needle
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6495
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         12093
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+12.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7476
_reflns_number_total             12093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01918a2.cif
_cod_data_source_block           Nickel_complex
_cod_depositor_comments
'Adding full bibliography for 7700880--7700883.cif.'
_cod_original_cell_volume        6367.3(16)
_cod_database_code               7700881
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C1B, F1B', F2B', F3B', C02S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1A, F2A, F3A, C4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1B, F1B, F2B, F3B, C4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4B, F5B, F6B, C3B, C5B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, F1A', F2A', F3A', C02I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C29B, C32B, F20B, F21B, F22B, F1, F2, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7A, F8A, F9A, C6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: F1A(0.5) F2A(0.5) F3A(0.5) C4A(0.5) F1A'(0.5) F2A'(0.5) F3A'(0.5)
 C02I(0.5) F4B(0.5) F5B(0.5) F6B(0.5) C5B(0.5) F1B(0.5) F2B(0.5) F3B(0.5)
 C4B(0.5) F1B'(0.5) F2B'(0.5) F3B'(0.5) C02S(0.5) F20B(0.5) F21B(0.5) F22B(0.5)
 F1(0.5) F2(0.5) F3(0.5) F5B'(0.5) F6B'(0.5) F4B'(0.5) C5B'(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C8A(H8A), C8B(H8B), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A), C27A(H27A), C28A(H28A), C30A(H30A), C34A(H34A), C35A(H35A),
 C36A(H36A), C37A(H37A), C38A(H38A), C20B(H20B), C21B(H21B), C22B(H22B),
 C23B(H23B), C27B(H27B), C28B(H28B), C30B(H30B), C34B(H34B), C35B(H35B),
 C36B(H36B), C37B(H37B), C38B(H38B)
;
_shelx_res_checksum              95565
_olex2_submission_special_instructions 'No special instructions were received'