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_2019968
_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_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      monoclinic
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_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
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_cell_angle_beta                 90.010(2)
_cell_angle_gamma                90
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_cell_length_b                   8.17630(10)
_cell_length_c                   22.1067(5)
_cell_measurement_reflns_used    79178
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      1.61
_cell_volume                     2783.01(9)
_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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<i>WinGX</i> (Farrugia, 2012), <i>publCIF</i> (Westrip, 2010)
and
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011)
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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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_diffrn_reflns_limit_h_min       -19
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;
(X-RED; Stoe & Cie, 2009)
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_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.210
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;
Flack <i>x</i> determined using 5183 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.037(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         12488
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.7358P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
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_reflns_number_gt                11928
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_cod_data_source_block           II-IT
_cod_database_code               2019968
_cod_database_fobs_code          2019968
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.971
_shelx_hkl_checksum              94567
_shelx_res_checksum              48785
_shelxl_version_number           .000002012