Ni(II) and Pd(II) complexes of a new redox-active pentadentate azo-appended 2-aminophenol ligand: Pd(II)-assisted intraligand cyclization forms a phenoxazinyl ring.
Bhowmik, Saumitra; Sengupta, Arunava; Mukherjee, Rabindranath; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14046–14064; doi:10.1039/d4dt01513d

data_7716740
_publ_section_title
;
 Ni(II) and Pd(II) complexes of a new redox-active pentadentate
 azo-appended 2-aminophenol ligand: Pd(II)-assisted intraligand
 cyclization forms a phenoxazinyl ring.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14046
_journal_page_last               14064
_journal_paper_doi               10.1039/d4dt01513d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H49 N4 Ni O2'
_chemical_formula_sum            'C40 H49 N4 Ni O2'
_chemical_formula_weight         676.52
_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             2021-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                71.713(2)
_cell_angle_beta                 81.597(2)
_cell_angle_gamma                89.058(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6539(7)
_cell_length_b                   11.1929(8)
_cell_length_c                   17.3192(12)
_cell_measurement_reflns_used    7104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.347
_cell_measurement_theta_min      2.824
_cell_volume                     1757.0(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33677
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_min         2.824
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             625
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.889
_exptl_transmission_factor_min   0.661
_refine_diff_density_max         1.582
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0295P)^2^+4.4330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7104
_reflns_number_total             8691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01513d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7716740--7716743.cif.'
_cod_database_code               7716740
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C16(H16), C22(H22), C23(H23), C13(H13), C7(H7), C34(H34), C25(H25),
 C24(H24), C19(H19), C18(H18), C17(H17)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C),
 C37(H37A,H37B,H37C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C4(H4A,H4B,H4C),
  C39(H39A,H39B,H39C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              46279
_shelx_hkl_checksum              67254
_olex2_submission_special_instructions 'No special instructions were received'