Phenoxazinyl Zn(II) diradical complex formed <i>via</i> redox-driven cyclization of a 2-aminophenol-based N<sub>3</sub>O ligand. Isolation of the modified N<sub>3</sub> ligand radical and its Ni(II) complex.
Mukhopadhyay, Narottam; Sengupta, Arunava; Lloret, Francesc; Mukherjee, Rabindranath; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6515–6519; doi:10.1039/d4dt00374h

data_7715600
_publ_section_title
;
 Phenoxazinyl Zn(II) diradical complex formed <i>via</i> redox-driven
 cyclization of a 2-aminophenol-based N<sub>3</sub>O ligand. Isolation of
 the modified N<sub>3</sub> ligand radical and its Ni(II) complex.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6515
_journal_page_last               6519
_journal_paper_doi               10.1039/d4dt00374h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'F6 Sb, 0.75(C H2 Cl2), C26 H29 N3 O2, 0.25[CH2Cl2]'
_chemical_formula_sum            'C26.75 H30.5 Cl1.5 F6 N3 O2 Sb'
_chemical_formula_weight         714.96
_chemical_name_systematic        '[H2L*]SBF6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                65.842(3)
_cell_angle_beta                 89.812(5)
_cell_angle_gamma                81.287(4)
_cell_formula_units_Z            8
_cell_length_a                   16.147(3)
_cell_length_b                   20.413(3)
_cell_length_c                   20.582(4)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.027
_cell_measurement_theta_min      2.343
_cell_volume                     6105.5(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21549
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.343
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0816 after correction.
The Ratio of minimum to maximum transmission is 0.7852.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       plate
_exptl_crystal_F_000             2868
_exptl_crystal_recrystallization_method 'Slow evaporation and layering'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.013
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.0027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1538
_refine_ls_number_reflns         21549
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1039P)^2^+56.3610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15999
_reflns_number_total             21549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00374h2.cif
_cod_data_source_block           PhZ
_cod_depositor_comments
'Adding full bibliography for 7715598--7715600.cif.'
_cod_original_cell_volume        6105.4(18)
_cod_original_formula_sum        'C26.75 H30.50 Cl1.50 F6 N3 O2 Sb'
_cod_database_code               7715600
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.810
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7013(17)
 0.2987(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C97-C98 \\sim C97-C98A
 with sigma of 0.02
 C97-C100 \\sim C97-C108
 with sigma of 0.02
 C97-C99 \\sim C97-C99A
 with sigma of 0.02
 C47-C45 \\sim C47A-C45
 with sigma of 0.02
 C45-C46 \\sim C45-C46A
 with sigma of 0.02
 C45-C48 \\sim C45-C48A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.2 and sigma
for terminal atoms of 0.02 within 1.7A
Uanis(C103) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
5. Others
 Sof(C99A)=Sof(H99d)=Sof(H99e)=Sof(H99f)=Sof(C98A)=Sof(H98d)=Sof(H98e)=
 Sof(H98f)=Sof(C108)=Sof(H10m)=Sof(H10n)=Sof(H10o)=1-FVAR(1)
 Sof(C98)=Sof(H98a)=Sof(H98b)=Sof(H98c)=Sof(C100)=Sof(H10j)=Sof(H10k)=
 Sof(H10l)=Sof(C99)=Sof(H99a)=Sof(H99b)=Sof(H99c)=FVAR(1)
 Sof(C47A)=Sof(H47d)=Sof(H47e)=Sof(H47f)=Sof(C48A)=Sof(H48d)=Sof(H48e)=
 Sof(H48f)=Sof(C46A)=Sof(H46d)=Sof(H46e)=Sof(H46f)=1-FVAR(2)
 Sof(C47)=Sof(H47a)=Sof(H47b)=Sof(H47c)=Sof(C46)=Sof(H46a)=Sof(H46b)=Sof(H46c)=
 Sof(C48)=Sof(H48a)=Sof(H48b)=Sof(H48c)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C106(H10p,H10q), C107(H10r,H10s), C105(H10t,H10u)
6.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N3(H3), N8(H8a), N9(H9a), C87(H87), N11(H11), C86(H86), N5(H5),
 N2(H2), C9(H9), C34(H34), N6(H6), C62(H62), C36(H36), C60(H60), C8(H8),
 C10(H10), C88(H88), C61(H61), C4(H4), C40(H40), C35(H35), C16(H16), C92(H92),
 C3(H3a), C82(H82), C68(H68), C81(H81), C14(H14), C1(H1), C80(H80), C56(H56),
 C27(H27), C2(H2a), C79(H79), C94(H94), C42(H42), C66(H66), C55(H55), C53(H53),
 C30(H30), C54(H54), C29(H29), C28(H28)
6.c Idealised Me refined as rotating group:
 C104(H10a,H10b,H10c), C103(H10d,H10e,H10f), C77(H77a,H77b,H77c), C50(H50a,
 H50b,H50c), C78(H78a,H78b,H78c), C76(H76a,H76b,H76c), C24(H24a,H24b,H24c),
 C52(H52a,H52b,H52c), C20(H20a,H20b,H20c), C26(H26a,H26b,H26c), C22(H22a,H22b,
 H22c), C21(H21a,H21b,H21c), C102(H10g,H10h,H10i), C25(H25a,H25b,H25c),
 C72(H72a,H72b,H72c), C51(H51a,H51b,H51c), C73(H73a,H73b,H73c), C47(H47a,H47b,
 H47c), C74(H74a,H74b,H74c), C46(H46a,H46b,H46c), C98(H98a,H98b,H98c),
 C100(H10j,H10k,H10l), C48(H48a,H48b,H48c), C99(H99a,H99b,H99c), C99A(H99d,H99e,
 H99f), C98A(H98d,H98e,H98f), C108(H10m,H10n,H10o), C47A(H47d,H47e,H47f),
 C48A(H48d,H48e,H48f), C46A(H46d,H46e,H46f)
;
_shelx_res_checksum              51857
_olex2_date_sample_completion    2023-11-07
_olex2_date_sample_data_collection 2023-11-07
_olex2_date_sample_submission    2023-11-04
_olex2_exptl_crystal_mounting_method 'with oil'
_olex2_submission_original_sample_id L*
_olex2_submission_special_instructions 'No special instructions were received'