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_7718129
_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 O3 Sn, C2 H3 N, C1.43 N0.99'
_chemical_formula_sum            'C75.42 H93 N3.98 O3 Sn'
_chemical_formula_weight         1222.01
_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             2022-12-22
_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                 109.078(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8998(13)
_cell_length_b                   18.8654(16)
_cell_length_c                   22.6765(19)
_cell_measurement_reflns_used    26748
_cell_measurement_temperature    115
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      1.90
_cell_volume                     6832.7(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.1678
_diffrn_reflns_av_unetI/netI     0.1523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR(Rigaku,1995)
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             2590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.852
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         12475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0652P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6856
_reflns_number_total             12475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00100e2.cif
_cod_data_source_block           shelx_trans_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7718127--7718131.cif.'
_cod_database_code               7718129
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.920
_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: C1(0.75)
3.a Ternary CH refined with riding coordinates:
 C00V(H00V), C00X(H00X), C013(H013), C017(H017), C01D(H01E), C01H(H01J),
 C01M(H01R), C01R(H01)
3.b Secondary CH2 refined with riding coordinates:
 C01U(H2AA,HF), C01V(H3AA,HG), C021(H02D,H02E), C025(H02O,H02P)
3.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00E(H00E), C00G(H00G), C00I(H00I), C00K(H00K),
 C00O(H00O), C00R(H00R), C00Y(H00Y), C010(H010), C011(H011), C012(H012),
 C014(H014), C019(H019), C01B(H01D), C01F(H01I), C01I(H01K), C01P(H01Y),
 C01Z(H6AA), C026(H026)
3.d Idealised Me refined as rotating group:
 C01A(H01A,H01B,H01C), C01E(H01F,H01G,H01H), C01J(H01L,H01M,H01N), C01L(H01O,
 H01P,H01Q), C01N(H01S,H01T,H01U), C01O(H01V,H01W,H01X), C01Q(H01Z,H,HA),
 C01S(H0AA,HB,HC), C01T(H1AA,HD,HE), C01W(H4AA,HH,HI), C01X(H5AA,HJ,HK),
 C01Y(H7AA,HL,HM), C020(H02A,H02B,H02C), C022(H02F,H02G,H02H), C023(H02I,H02J,
 H02K), C024(H02L,H02M,H02N), C027(H02Q,H02R,H02S), C028(H02T,H02U,H02V),
 C029(H02W,H02X,H02Y)
;
_olex2_submission_special_instructions 'No special instructions were received'