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_2018736
_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          566
_chemical_name_systematic
;
(<i>RS</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           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                71.030(5)
_cell_angle_beta                 87.440(6)
_cell_angle_gamma                84.553(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3148(5)
_cell_length_b                   8.6633(5)
_cell_length_c                   12.4320(8)
_cell_measurement_reflns_used    35193
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      1.73
_cell_volume                     842.97(9)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0546
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13032
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.8656
_exptl_absorpt_correction_T_min  0.7444
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.812
_refine_diff_density_min         -2.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0553P)^2^+0.5942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                3798
_reflns_number_total             3859
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            eg3106.cif
_cod_data_source_block           II
_cod_database_code               2018736
_cod_database_fobs_code          2018736