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_7718127
_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         'C74 H88 N2 O Sn, C4 H8 O, C2 H3 N'
_chemical_formula_sum            'C80 H99 N3 O2 Sn'
_chemical_formula_weight         1253.31
_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             2023-03-21
_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                 101.332(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3796(8)
_cell_length_b                   18.5286(10)
_cell_length_c                   22.9413(10)
_cell_measurement_reflns_used    45190
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.965
_cell_volume                     7243.5(6)
_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
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66485
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.118
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         16437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0640
_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^)+22.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12403
_reflns_number_total             16437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00100e2.cif
_cod_data_source_block           shelx_trans
_cod_depositor_comments
'Adding full bibliography for 7718127--7718131.cif.'
_cod_database_code               7718127
_shelx_shelxl_version_number     2018/1
_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. Others
 Fixed Sof: N0AA(0.5) N3(0.5)
3.a Ternary CH refined with riding coordinates:
 C53(H53), C26(H26), C56(H56), C68(H68), C23(H23), C65(H65), C38(H38), C35(H35)
3.b Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C78(H78A,H78B), C77(H77A,H77B), C71(H71A,H71B), C76(H76A,
 H76B), C72(H72A,H72B), C74(H74A,H74B), C73(H73A,H73B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C46(H46), C42(H42), C44(H44), C12(H12), C50(H50), C7(H7),
 C51(H51), C19(H19), C4(H4), C16(H16), C49(H49), C5(H5), C6(H6), C21(H21),
 C20(H20), C63(H63), C14(H14), C62(H62), C61(H61), C33(H33), C32(H32), C31(H31)
3.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C69(H69A,H69B,
 H69C), C57(H57A,H57B,H57C), C25(H25A,H25B,H25C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C27(H27A,H27B,H27C), C70(H70A,H70B,H70C), C28(H28A,H28B,H28C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C58(H58A,H58B,H58C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C), C80(H80A,H80B,H80C)
;
_olex2_submission_special_instructions 'No special instructions were received'