Novel Stannatrane N(CH2CMe2O)2(CMe2CH2O)SnO-t-Bu and Related Oligonuclear Tin(IV) Oxoclusters. Two Isomers in One Crystal.
Glowacki, Britta; Lutter, Michael; Schollmeyer, Dieter; Hiller, Wolf; Jurkschat, Klaus; Inorganic chemistry  (2016) –; doi:10.1021/acs.inorgchem.6b01429

data_4344911
_publ_section_title
;
 Novel Stannatrane N(CH2CMe2O)2(CMe2CH2O)SnO-t-Bu and Related Oligonuclear
 Tin(IV) Oxoclusters. Two Isomers in One Crystal.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b01429
_journal_year                    2016
_chemical_formula_moiety
'2 (C40 H81 N3 O11 Sn3), 0.5 (C7 H8), 0.5 (C7 H8)'
_chemical_formula_sum            'C83.5 H166 N6 O22 Sn6'
_chemical_formula_weight         2318.35
_chemical_melting_point          458
_chemical_name_systematic
;
(m3-oxido)(tert-Butanolato)-tris(2,8,9-trioxa-5-aza-3,3,7,7,11,11-
tetramethyl-1-stanna-tricyclo[3.3.3.01,5]-undecane) 
(m3-oxido)(m3-tert-Butanolato)-tris(2,8,9-trioxa-5-aza-3,3,7,7,11,11-
tetramethyl-1-stanna-tricyclo[3.3.3.01,5]-undecane)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                115.0897(19)
_cell_angle_beta                 90.2795(16)
_cell_angle_gamma                103.5550(16)
_cell_formula_units_Z            2
_cell_length_a                   13.2531(2)
_cell_length_b                   20.4541(4)
_cell_length_c                   21.7910(4)
_cell_measurement_reflns_used    39914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.7750
_cell_measurement_theta_min      2.4760
_cell_volume                     5164.13(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    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0560
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             2370
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.386
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         19207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.386
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16893
_reflns_number_total             19207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01429_si_001.cif
_cod_data_source_block           comp3
_cod_original_cell_volume        5164.14(19)
_cod_original_formula_sum        'C83.50 H166 N6 O22 Sn6'
_cod_database_code               4344911
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.754
_shelx_res_checksum              8038
_shelx_hkl_checksum              28997