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_7715599
_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         'C52 H54 N6 Ni O4'
_chemical_formula_sum            'C52 H54 N6 Ni O4'
_chemical_formula_weight         885.72
_chemical_name_systematic        '[Ni(L*)2]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-23 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.049(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.392(3)
_cell_length_b                   17.272(3)
_cell_length_c                   23.289(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.327
_cell_measurement_theta_min      2.566
_cell_volume                     9189(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_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  0.0713
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63664
_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         26.368
_diffrn_reflns_theta_min         2.566
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1063 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.9269.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_preparation       'Layering of n-Hexane in DCM'
_exptl_crystal_recrystallization_method 'Layering of n-Hexane in DCM'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0311P)^2^+12.8573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7230
_reflns_number_total             9399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00374h2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7715598--7715600.cif.'
_cod_database_code               7715599
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C27(H27), C4(H4), C8(H8), C16(H16), C40(H40), C14(H14), C1(H1),
 C3(H3), C35(H35), C9(H9), C34(H34), C28(H28), C36(H36), C42(H42), C10(H10),
 C29(H29), C30(H30)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C46(H46A,
 H46B,H46C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C), C50(H50A,H50B,H50C),
 C47(H47A,H47B,H47C)
;
_shelx_res_checksum              66113
_olex2_date_sample_completion    2023-11-10
_olex2_date_sample_data_collection 2023-11-10
_olex2_date_sample_submission    2023-11-08
_olex2_exptl_crystal_mounting_method 'In oil'
_olex2_submission_original_sample_id 'Complex 2'
_olex2_submission_special_instructions 'No special instructions were received'