Complexity of imine and amine Schiff-base tin(ii) complexes: drastic differences of amino and pyridyl side arms
Yimthachote, Supajittra; Chumsaeng, Phongnarin; Phomphrai, Khamphee; Dalton Transactions  (2021) –; doi:10.1039/D1DT02997E

data_7708965
_publ_section_title
;
 Complexity of imine and amine Schiff-base tin(ii) complexes: drastic
 differences of amino and pyridyl side arms
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02997E
_journal_year                    2021
_chemical_formula_moiety         'C27 H45 N3 O Si2 Sn'
_chemical_formula_sum            'C27 H45 N3 O Si2 Sn'
_chemical_formula_weight         602.53
_chemical_name_systematic        1b
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-12 deposited with the CCDC.	2021-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.329(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3321(9)
_cell_length_b                   20.111(2)
_cell_length_c                   18.170(2)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.32
_cell_volume                     3039.6(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            139438
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.246
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0577 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.9008.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull light green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7251
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+2.8477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6897
_reflns_number_total             7251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02997e2.cif
_cod_data_source_block           p21_n
_cod_original_cell_volume        3039.5(6)
_cod_database_code               7708965
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.715
_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. Restrained distances
 Si2-N3 \\sim Si2A-N3
 with sigma of 0.02
 C26-C25 \\sim C26A-C25A
 with sigma of 0.04
 N3-C25 \\sim N3-C25A
 with sigma of 0.04
 N3-C27 \\sim N3-C27A
 with sigma of 0.04
 C27-C25 \\sim C27A-C25A
 with sigma of 0.04
 N3-C26 \\sim N3-C26A
 with sigma of 0.04
 C27-C26 \\sim C27A-C26A
 with sigma of 0.04
 Si2-C25 \\sim Si2A-C25A
 with sigma of 0.02
 Si2-C27 \\sim Si2A-C27A
 with sigma of 0.02
 Si2-C26 \\sim Si2A-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27A \\sim C27: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C25 \\sim C25A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C26 \\sim C26A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C27) = Uanis(C27A)
Uanis(C25) = Uanis(C25A)
4. Rigid body (RIGU) restrains
 Si2, C26, C25, C27, Si2A, C26A, C25A, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(Si2A)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(Si2)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C),
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F)
;
_shelx_res_checksum              56358
_shelx_hkl_checksum              25404
_olex2_submission_special_instructions 'No special instructions were received'