cyclo-Stannasiloxanes Containing both Oxygen Atoms and Methylene Moieties within the Ring and Formation of Related Organotin Oxo Clusters
Baba Haj, Samer; Dietz, Christina; Lutter, Michael; Jurkschat, Klaus; Organometallics 34 (2015) 5555–; doi:10.1021/acs.organomet.5b00768

data_4087969
_publ_section_title
;
 cyclo-Stannasiloxanes Containing both Oxygen Atoms and Methylene Moieties
 within the Ring and Formation of Related Organotin Oxo Clusters
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5555
_journal_paper_doi               10.1021/acs.organomet.5b00768
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C22 H52 O2 Si2 Sn2'
_chemical_formula_sum            'C22 H52 O2 Si2 Sn2'
_chemical_formula_weight         642.19
_chemical_melting_point          106.5(10)
_chemical_name_common            cyclo-(t-Bu2SnOMe2SiCH2)2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.908(4)
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_cell_measurement_reflns_used    9670
_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.5428
_cell_volume                     747.32(7)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
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'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'enCIFer Version 1.5'
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_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8852
_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         25.499
_diffrn_reflns_theta_min         2.548
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57851
_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    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.348
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0262P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2681
_reflns_number_total             2773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00768_si_002.cif
_cod_data_source_block           comp6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '105.5-107.5' was changed
to '106.5(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4087969
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.472
_shelx_estimated_absorpt_t_max   0.594
_shelx_res_checksum              37748
_shelx_hkl_checksum              40189