Dichloridobis{2-[(dimethylamino)methyl]phenyl}bis{2-[(dimethylazaniumyl)methyl]phenyl}di-μ-hydroxido-di-μ~3~-oxido-tetraphenyltetratin(IV) dichloride deuterochloroform decasolvate
Turek, Jan; Padělková, Zdeňka; Acta Crystallographica Section E 67 (2011) m1890–m1891; doi:10.1107/S1600536811048872

data_2232548
_publ_section_title
;
 Dichloridobis{2-[(dimethylamino)methyl]phenyl}bis{2-[(dimethylazaniumyl)methyl]phenyl}di-\m-hydroxido-di-\m~3~-oxido-tetraphenyltetratin(IV)
 dichloride deuterochloroform decasolvate
;
_journal_coeditor_code           AA2022
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1890
_journal_page_last               m1891
_journal_paper_doi               10.1107/S1600536811048872
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Sn4 (C6 H5)4 Cl2 O2 (O H)2 (C9 H13 N1)2 (C9 H12 N1)2] Cl2, 10C D Cl3'
_chemical_formula_moiety
'C60 H72 Cl2 N4 O4 Sn4 2+, 2(Cl -), 10(C D Cl3)'
_chemical_formula_sum            'C70 H72 Cl34 D10 N4 O4 Sn4'
_chemical_formula_weight         2733.56
_chemical_melting_point          395(2)
_chemical_name_common
;
Dichloridobis{2-[(dimethylamino)methyl]phenyl}bis{2-
[(dimethylazaniumyl)methyl]phenyl}di-\m-hydroxido-di-\m~3~-oxido-
tetraphenyltetratin(IV) dichloride deuterochloroform decasolvate
;
_chemical_name_systematic
;
bis{2-[2-(dimethylazaniumyl)methyl]phenyl}-2\k<i>C</i>^1^,3\k<i>C</i>^1^-
bis{2-[(dimethylamino)methyl]phenyl}-1\k<i>C</i>^1^,4\k<i>C</i>^1^-
dichlorido-1\k<i>Cl</i>,4\k<i>Cl</i>-
di-\m-hydroxido-1:2\k^2^<i>O</i>:<i>O</i>;3:4\k^2^<i>O</i>:<i>O</i>-
di-\m~3~-oxido-1:2:3\k^3^<i>O</i>:<i>O</i>:<i>O</i>;2:3:4\k^3^<i>O</i>:
<i>O</i>:<i>O</i>-tetraphenyl-
1\k<i>C</i>^1^,2\k<i>C</i>^1^,3\k<i>C</i>^1^,4\k<i>C</i>^1^-tetratin(IV)
dichloride deuterochloroform decasolvate
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                83.752(7)
_cell_angle_beta                 68.178(4)
_cell_angle_gamma                76.339(5)
_cell_formula_units_Z            1
_cell_length_a                   11.9279(5)
_cell_length_b                   15.4080(12)
_cell_length_c                   15.9651(14)
_cell_measurement_reflns_used    51386
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2646.1(3)
_computing_cell_refinement
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            51386
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         12052
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+12.7718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                9459
_reflns_number_total             12052
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            aa2022.cif
_cod_data_source_block           I
_cod_database_code               2232548
_cod_database_fobs_code          2232548