Insights into the Hydrolytic Polymerization of Trimethoxymethylsilane. Crystal Structure of (MeO)2MeSiONa.
Richers, Casseday P.; Bertke, Jeffery; Rauchfuss, Thomas B.; Inorganic chemistry 55 (2016) 5744–5746; doi:10.1021/acs.inorgchem.6b00874

data_4348023
_publ_contact_author
; 
Thomas B. Rauchfuss
Department of Chemistry
University of Illinois 
A328 CLSL, Box 12-6 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Insights into the Hydrolytic Polymerization of Trimethoxymethylsilane.
 Crystal Structure of (MeO)2MeSiONa.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5744
_journal_page_last               5746
_journal_paper_doi               10.1021/acs.inorgchem.6b00874
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C3 H9 O3 Si -, 0.4(C H4 O), Na+'
_chemical_formula_sum            'C3.4 H10.6 Na O3.4 Si'
_chemical_formula_weight         156.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                85.639(6)
_cell_angle_beta                 82.851(5)
_cell_angle_gamma                66.091(5)
_cell_formula_units_Z            10
_cell_length_a                   11.5098(12)
_cell_length_b                   12.9494(14)
_cell_length_c                   14.6016(16)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.31
_cell_volume                     1973.3(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm51qsa
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43275
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.526
_diffrn_reflns_theta_min         2.192
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.98912
_exptl_absorpt_correction_T_min  0.94041
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_id                cm51qsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 -1 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8199
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0491P)^2^+1.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7451
_reflns_number_total             8199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00874_si_002.cif
_cod_data_source_block           cm51qsa
_cod_depositor_comments
;

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C17 H53 Na5 O17 Si5'
_cod_original_formula_weight         784.99
_cod_original_formula_moiety         'C17 H53 Na5 O17 Si5 '
_cod_original_formula_units_Z            2
_cod_database_code               4348023
_shelx_estimated_absorpt_t_min   0.885
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2014/6
_shelx_res_checksum              88213
_shelx_hkl_checksum              68242