Enantiotropic phase transition in a binuclear tin complex with an <i>O</i>,<i>N</i>,<i>O</i>'-tridentate ligand
Schwarzer, Anke; Paul, Lydia E. H.; Böhme, Uwe; Acta Crystallographica Section C 69 (2013) 1336–1339; doi:10.1107/S0108270113027194

data_2019261
_publ_section_title
;
 Enantiotropic phase transition in a binuclear tin complex with an
 <i>O</i>,<i>N</i>,<i>O</i>'-tridentate ligand
;
_journal_coeditor_code           YP3047
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1336
_journal_page_last               1339
_journal_paper_doi               10.1107/S0108270113027194
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Sn2 (C2 H3)3 (C9 H9 N O2)2 Cl]'
_chemical_formula_moiety         'C24 H27 Cl N2 O4 Sn2'
_chemical_formula_sum            'C24 H27 Cl N2 O4 Sn2'
_chemical_formula_weight         680.31
_chemical_name_systematic
Chlorido{\m-2-[(2-oxidobenzylidene)amino]ethan-1-olato-\k^4^<i>O</i>,<i>N</i>,<i>O</i>':<i>O</i>'}{2-[(2-oxidobenzylidene)amino]ethan-1-olato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>'}trivinylditin(IV)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.3350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5649(3)
_cell_length_b                   15.9508(4)
_cell_length_c                   13.3525(3)
_cell_measurement_reflns_used    5961
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.55
_cell_volume                     2623.91(11)
_computing_cell_refinement       'SMART (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23707
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.7777
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.598
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0335P)^2^+1.1976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                4378
_reflns_number_total             6341
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yp3047.cif
_cod_data_source_block           III-HT
_cod_original_cell_volume        2623.91(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019261