Two reversible enantiotropic phase transitions in a pentacoordinate silicon complex with an <i>O</i>,<i>N</i>,<i>O</i>'-tridentate valinate ligand
Schwarzer, Anke; Fels, Sabine; Böhme, Uwe; Acta Crystallographica Section C 71 (2015) 511–516; doi:10.1107/S2053229615009778

data_2019967
_publ_section_title
;
 Two reversible enantiotropic phase transitions in a pentacoordinate
 silicon complex with an <i>O</i>,<i>N</i>,<i>O</i>'-tridentate valinate
 ligand
;
_journal_coeditor_code           EG3182
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              511
_journal_page_last               516
_journal_paper_doi               10.1107/S2053229615009778
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C12 H21 N O3 Si'
_chemical_formula_moiety         'C12 H21 N O3 Si'
_chemical_formula_sum            'C12 H21 N O3 Si'
_chemical_formula_weight         255.39
_chemical_name_common
;
(3S)-5,7,9,9-tetramethyl-3-(propan-2-yl)-2H,3H,9H-1,8,4\l^4^,\
\l^5^-[1,3\l^4^,2\l^5^]oxazasilolo[2,3-b][1,3\l^4^,2\l^5^]oxazasilin-2-one
;
_chemical_name_systematic
Dimethyl[<i>N</i>-(4-oxidopent-3-en-2-ylidene)valinato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>']silicon(II)
_space_group_crystal_system      orthorhombic
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   8.1899(2)
_cell_length_c                   22.0975(6)
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_cell_measurement_temperature    203(2)
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_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
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X-RED (Stoe & Cie, 2009)
;
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ORTEP-3 for Windows (Farrugia, 2012)
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SHELXL2014 (Sheldrick, 2015)
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SHELXL2014 (Sheldrick, 2015)
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SHELXS97 (Sheldrick, 2008)
;
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_diffrn_measurement_device       '2-circle goniometer'
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;
(X-RED; Stoe & Cie, 2009)
;
_exptl_crystal_colour            Colourless
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_exptl_crystal_description       Prism
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_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.560
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1174 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3236
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_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.8892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     I>2\s(I)
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_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.971
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