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_7718131
_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         'C70 H84 Cl2 N2 O Sn, C2 H3 N, C4 O'
_chemical_formula_sum            'C76 H87 Cl2 N3 O2 Sn'
_chemical_formula_weight         1264.07
_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                 106.496(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3591(7)
_cell_length_b                   18.5527(9)
_cell_length_c                   22.2644(9)
_cell_measurement_reflns_used    95647
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6875.3(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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'R-AXIS RAPID'
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            65637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.201
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.496
_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    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         15700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0447P)^2^+12.9486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13387
_reflns_number_total             15700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00100e2.cif
_cod_data_source_block           shelx_trans_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7718127--7718131.cif.'
_cod_database_code               7718131
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.790
_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: C73(0.75) C75(0.25)
3.a Ternary CH refined with riding coordinates:
 C49(H49), C52(H52), C22(H22), C19(H19), C64(H64), C34(H34), C31(H31), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C12(H12), C8(H8), C38(H38), C42(H42), C10(H10), C40(H40),
 C17(H17), C47(H47), C45(H45), C59(H59), C46(H46), C16(H16), C15(H15), C29(H29),
  C58(H58), C28(H28), C57(H57), C27(H27)
3.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C21(H21A,H21B,H21C), C50(H50A,H50B,
 H50C), C20(H20A,H20B,H20C), C66(H66A,H66B,H66C), C65(H65A,H65B,H65C), C35(H35A,
 H35B,H35C), C53(H53A,H53B,H53C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C),
 C32(H32A,H32B,H32C), C77(H77A,H77B,H77C), C23(H23A,H23B,H23C), C33(H33A,H33B,
 H33C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_olex2_submission_special_instructions 'No special instructions were received'