Enantiomerically pure and racemic dimethyl{<i>N</i>-[(2-oxidonaphthalen-1-yl-κ<i>O</i>)methylidene]valinato-κ^2^<i>N</i>,<i>O</i>}tin(IV)
Böhme, Uwe; Fels, Sabine; Acta Crystallographica Section C 69 (2013) 44–46; doi:10.1107/S0108270112050470

data_2018735
_publ_section_title
;
 Enantiomerically pure and racemic
 dimethyl{<i>N</i>-[(2-oxidonaphthalen-1-yl-\k<i>O</i>)methylidene]valinato-\k^2^<i>N</i>,<i>O</i>}tin(IV)
;
_journal_coeditor_code           EG3106
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              44
_journal_page_last               46
_journal_paper_doi               10.1107/S0108270112050470
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Sn (C H3)2 (C16 H15 N O3)]'
_chemical_formula_moiety         'C18 H21 N O3 Sn'
_chemical_formula_sum            'C18 H21 N O3 Sn'
_chemical_formula_weight         418.05
_chemical_melting_point          514
_chemical_name_systematic
;
(<i>S</i>)-Dimethyl{<i>N</i>-[(2-oxidonaphthalen-1-yl-
\k<i>O</i>)methylidene]valinato-\k^2^<i>N</i>,<i>O</i>}tin(IV)
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.6246(5)
_cell_length_b                   11.6246(5)
_cell_length_c                   11.5864(5)
_cell_measurement_reflns_used    24695
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.68
_cell_volume                     1355.92(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2009'
_computing_data_collection       'X-AREA (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2009'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       '\f rotation 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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14770
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.7833
_exptl_absorpt_correction_T_min  0.5992
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2009'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.391
_refine_diff_density_min         -1.069
_refine_ls_abs_structure_details 'Flack (1983), <b>???? Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.0805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                4082
_reflns_number_total             4140
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            eg3106.cif
_cod_data_source_block           I
_cod_database_code               2018735
_cod_database_fobs_code          2018735