Penta- and hexaorganostannate(iv) complexes based on O-heterocyclic ligands
Gebauer, Ireen; Gräsing, Daniel; Matysik, Jörg; Zahn, Stefan; Zeckert, Kornelia; Dalton Trans.  (2017) –; doi:10.1039/C7DT01336A

data_7043355
_publ_section_title
;
 Penta- and hexaorganostannate(iv) complexes based on O-heterocyclic
 ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01336A
_journal_year                    2017
_chemical_formula_moiety         'C72 H78 K2 O12 Sn, C64 H62 K2 O10 Sn'
_chemical_formula_sum            'C136 H140 K4 O22 Sn2'
_chemical_formula_weight         2520.26
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2016-09-12T10:05:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.033(3)
_cell_angle_beta                 93.473(3)
_cell_angle_gamma                109.331(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3438(4)
_cell_length_b                   16.2908(6)
_cell_length_c                   17.5765(7)
_cell_measurement_reflns_used    6350
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.622
_cell_measurement_theta_min      2.696
_cell_volume                     3004.8(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
            SHELXS-97
            Program for Crystal Structure Analysis (Release 97-2)
            G. M. Sheldrick, Institut f\"ur Anorganische Chemie der Universit\"at,
            Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.356
_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, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0052467
_diffrn_orient_matrix_UB_12      -0.0126705
_diffrn_orient_matrix_UB_13      0.0365125
_diffrn_orient_matrix_UB_21      0.0647397
_diffrn_orient_matrix_UB_22      0.0264826
_diffrn_orient_matrix_UB_23      0.006421
_diffrn_orient_matrix_UB_31      -0.0153964
_diffrn_orient_matrix_UB_32      0.0366761
_diffrn_orient_matrix_UB_33      0.0178888
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23588
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.92876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         12285
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.7581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                8604
_reflns_number_total             12285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01336a2.cif
_cod_data_source_block           x2334
_cod_original_cell_volume        3004.84(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7043355