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_7718128
_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         'C38 H46 N2 O Sn'
_chemical_formula_sum            'C38 H46 N2 O Sn'
_chemical_formula_weight         665.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5302(8)
_cell_length_b                   31.242(2)
_cell_length_c                   11.5295(10)
_cell_measurement_reflns_used    30040
_cell_measurement_temperature    158
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      .033
_cell_volume                     3432.8(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      158
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30040
_diffrn_reflns_theta_full        27.4826
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.775
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2876
_exptl_crystal_description       needle
_exptl_crystal_F_000             1381.9637
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.4947
_refine_diff_density_min         -2.5259
_refine_diff_density_rms         0.2002
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             7.8105
_refine_ls_goodness_of_fit_ref   1.0394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0394
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+16.5660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              40
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3248
_reflns_number_total             4006
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt00100e2.cif
_cod_data_source_block           shelx_trans_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7718127--7718131.cif.'
_cod_database_code               7718128
_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
2. Others
 Fixed Sof: C22(0.5) C21(0.25) C23(0.2) C20(0.15) C18(0.6) C19(0.3)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C5(H5), C2(H2), C3(H3)
3.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C13(H13a,H13b,H13c), C12(H12a,H12b,
 H12c), C11(H11a,H11b,H11c), C15(H15a,H15b,H15c)
;
_olex2_submission_special_instructions 'No special instructions were received'