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_7700882
_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 O4 Zn'
_chemical_formula_sum            'C29 H14 F15 N4 O4 Zn'
_chemical_formula_weight         832.81
_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-alpha
(compiled 2018.01.22 svn.r3481 for OlexSys, GUI svn.r5457)
;
_audit_update_record
;
2018-12-02 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.370(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7227(8)
_cell_length_b                   23.2862(14)
_cell_length_c                   20.7274(11)
_cell_measurement_reflns_used    9072
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      21.979
_cell_measurement_theta_min      2.221
_cell_volume                     6386.5(6)
_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)'
_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_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11233
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.770
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0629 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.9078. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         11233
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0870P)^2^+15.8326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7168
_reflns_number_total             11233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01918a2.cif
_cod_data_source_block           Zinc_complex
_cod_depositor_comments
'Adding full bibliography for 7700880--7700883.cif.'
_cod_database_code               7700882
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.880(3)
 0.120(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C1B-C9 \\sim C1B-C1AA
 with sigma of 0.02
 F1B-C9 \\sim F1C-C1AA
 with sigma of 0.02
 F3B-C9 \\sim F3C-C1AA
 with sigma of 0.02
 F2B-C9 \\sim F2C-C1AA
 with sigma of 0.02
 C1B-F1B \\sim C1B-F1C
 with sigma of 0.04
 C1B-F3B \\sim C1B-F3C
 with sigma of 0.04
 C1B-F2B \\sim C1B-F2C
 with sigma of 0.04
 F1B-F3B \\sim F1C-F3C
 with sigma of 0.04
 F1B-F2B \\sim F1C-F2C
 with sigma of 0.04
 F3B-F2B \\sim F3C-F2C
 with sigma of 0.04
 F4B-C5B \\sim F6B'-C5B'
 with sigma of 0.02
 F5B-C5B \\sim F4B'-C5B'
 with sigma of 0.02
 F6B-C5B \\sim F5B'-C5B'
 with sigma of 0.02
 C3B-C5B \\sim C3B-C5B'
 with sigma of 0.02
 F4B-F5B \\sim F6B'-F4B'
 with sigma of 0.04
 F4B-F6B \\sim F6B'-F5B'
 with sigma of 0.04
 F4B-C3B \\sim F6B'-C3B
 with sigma of 0.04
 F5B-F6B \\sim F4B'-F5B'
 with sigma of 0.04
 F5B-C3B \\sim F4B'-C3B
 with sigma of 0.04
 F6B-C3B \\sim F5B'-C3B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(F1C) \\sim Ueq, Uanis(F3C) \\sim Ueq, Uanis(F2C) \\sim Ueq, Uanis(C1AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1B) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 F1, F2, F3, C32B, C29B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1B, F3B, F2B, C9, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1B, F1C, F2C, F3C, C1AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F6B', F4B', F5B', C5B', C3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32B, F20B, F21B, F22B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4B, F5B, F6B, C5B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1C, F3C, F2C, C1AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1B, F3B, F2B, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: F4B(0.5) F5B(0.5) F6B(0.5) C5B(0.5) F20B(0.5) F21B(0.5) F22B(0.5)
 F1(0.5) F2(0.5) F3(0.5) F1B(0.5) F3B(0.5) F2B(0.5) C9(0.5) F1C(0.5) F3C(0.5)
 F2C(0.5) C1AA(0.5) F6B'(0.5) F4B'(0.5) F5B'(0.5) C5B'(0.5)
7.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              93340
_olex2_submission_special_instructions 'No special instructions were received'