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_2019969
_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      orthorhombic
_space_group_IT_number           19
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   22.9355(7)
_cell_length_b                   8.1571(2)
_cell_length_c                   22.1230(5)
_cell_measurement_reflns_used    43033
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      1.28
_cell_volume                     4138.93(19)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
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X-AREA (Stoe & Cie, 2009)
;
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X-RED (Stoe & Cie, 2009)
;
_computing_molecular_graphics
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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'
_diffrn_measurement_device_type  'Stoe IPDS 2'
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_diffrn_radiation_monochromator  'plane graphite'
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_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43033
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         1.841
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.8290
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;
(X-RED; Stoe & Cie, 2009)
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_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.230
_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
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;
Flack <i>x</i> determined using 3434 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.7433P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                8495
_reflns_number_total             9511
_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           II-LT
_cod_database_code               2019969
_cod_database_fobs_code          2019969
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              98882
_shelx_res_checksum              86362
_shelxl_version_number           .000002012