Redox-active tin(II) complexes with sterically demanding <i>o</i>-phenylenediamido ligands and their reactivity with organic azides.
Sugimoto, Hideki; Yoneda, Akira; Yano, Mayuka; Sato, Kazunobu; Shiota, Yoshihito; Miyanishi, Mayuko; Yoshizawa, Kazunari; Itoh, Shinobu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5025–5034; doi:10.1039/d5dt00100e

data_7718130
_publ_section_title
;
 Redox-active tin(II) complexes with sterically demanding
 <i>o</i>-phenylenediamido ligands and their reactivity with organic
 azides.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5025
_journal_page_last               5034
_journal_paper_doi               10.1039/d5dt00100e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C72 H90 N2 O Sn, 2(C2 H3 N)'
_chemical_formula_sum            'C76 H96 N4 O Sn'
_chemical_formula_weight         1200.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-12 deposited with the CCDC.	2025-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.608(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0941(9)
_cell_length_b                   18.8683(11)
_cell_length_c                   22.2358(12)
_cell_measurement_reflns_used    57625
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6872.7(7)
_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      115.0
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57617
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.075
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.416
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         15674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+1.1720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12087
_reflns_number_total             15674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00100e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7718127--7718131.cif.'
_cod_database_code               7718130
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C54(H54), C24(H24), C51(H51), C21(H21), C36(H36), C33(H33), C66(H66), C63(H63)
2.b Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C5(H5), C14(H14), C44(H44), C10(H10), C2(H2), C12(H12), C19(H19),
 C49(H49), C42(H42), C18(H18), C17(H17), C31(H31), C47(H47), C48(H48), C29(H29),
  C30(H30), C61(H61), C59(H59), C60(H60)
2.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C),
 C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C23(H23A,H23B,H23C), C37(H37A,H37B,
 H37C), C52(H52A,H52B,H52C), C22(H22A,H22B,H22C), C68(H68A,H68B,H68C), C25(H25A,
 H25B,H25C), C65(H65A,H65B,H65C), C35(H35A,H35B,H35C), C76(H76A,H76B,H76C),
 C67(H67A,H67B,H67C), C38(H38A,H38B,H38C), C64(H64A,H64B,H64C), C34(H34A,H34B,
 H34C), C74(H74A,H74B,H74C)
;
_olex2_submission_special_instructions 'No special instructions were received'