Novel Trialkanolamine Derivatives of Tin of the Type [N(CH2CMe2O)2(CH2)nOSnOR]m (m= 1, 2;n= 2, 3; R =t-Bu, 2,6-Me2C6H3) and Related Tri- and Pentanuclear Tin(IV) Oxoclusters. Syntheses and Molecular Structures
Thomas Zöller; Klaus Jurkschat; Inorganic Chemistry 52 (2013) 1872–1882; doi:10.1021/ic302042n

data_4333814
_publ_contact_author_address
;Technische Universit\"at Dortmund
Otto-Hahn-Stra\&se 6
Lehrstuhl f\"ur Anorganische Chemie II
44227 Dortmund
;
_publ_contact_author_email       klaus.jurkschat@tu-dortmund.de
_publ_contact_author_name        'Klaus Jurkschat'
_publ_section_title
;
 Novel Trialkanolamine Derivatives of Tin of the Type
 [N(CH2CMe2O)2(CH2)nOSnOR]m (m= 1, 2;n= 2, 3; R =t-Bu, 2,6-Me2C6H3) and
 Related Tri- and Pentanuclear Tin(IV) Oxoclusters. Syntheses and
 Molecular Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1872
_journal_page_last               1882
_journal_paper_doi               10.1021/ic302042n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H62 N2 O8 Sn2, C7 H8'
_chemical_formula_sum            'C37 H70 N2 O8 Sn2'
_chemical_formula_weight         908.33
_chemical_melting_point          533
_chemical_name_systematic
; 
Bis{1-tert-butanolato-(2,9,10-trioxa-6-aza-8,8,11,11-
tetramethylstannatricyclo-[4.3.3.0^1.6^]dodecane} toluene solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.230(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8063(6)
_cell_length_b                   12.5549(6)
_cell_length_c                   14.1181(8)
_cell_measurement_reflns_used    5106
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1580
_cell_measurement_theta_min      2.1920
_cell_volume                     2045.19(19)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur2 CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9050
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0499
_reflns_number_gt                2885
_reflns_number_total             3800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302042n_si_002_3.cif
_cod_data_source_block           1639_compound4*toluene
_cod_original_cell_volume        2045.19(18)
_cod_database_code               4333814