Intramolecularly Coordinated Bis(crown ether)-Substituted Organotin Halides as Ditopic Salt Receptors
Arens, Verena; Dietz, Christina; Schollmeyer, Dieter; Jurkschat, Klaus; Organometallics 32 (2013) 2775–; doi:10.1021/om400216z

data_4080816
_publ_section_title
;
 Intramolecularly Coordinated Bis(crown ether)-Substituted Organotin
 Halides as Ditopic Salt Receptors
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2775
_journal_paper_doi               10.1021/om400216z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C24 H46 Cl2 O10 Sn'
_chemical_formula_sum            'C24 H46 Cl2 O10 Sn'
_chemical_formula_weight         684.20
_chemical_melting_point          409
_chemical_name_systematic
; 
dichlorido-bis(1,4,7,10,13-pentaoxacyclohexadec-15-ylmethyl)-stannane 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 100.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.948(4)
_cell_length_b                   11.4212(6)
_cell_length_c                   16.389(2)
_cell_measurement_reflns_used    4734
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1022
_cell_measurement_theta_min      2.1805
_cell_volume                     2938.1(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12808
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98409
_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    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0360
_reflns_number_gt                2094
_reflns_number_total             2745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400216z_si_001.cif
_cod_data_source_block           compound5_1128ia
_cod_original_cell_volume        2938.1(8)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4080816