Tetraalkylammonium pentaorganosilicates: the first highly stable silicates with five hydrocarbon ligands
Deerenberg, Sirik; Schakel, Marius; Keijzer, Adrianus H. J. F. de; Kranenburg, Mirko; Lutz, Martin; Spek, Anthony L.; Lammertsma, Koop; Chemical Communications  (2002) 348–; doi:10.1039/b109816k

data_7114104
_publ_section_title
;
 Tetraalkylammonium pentaorganosilicates: the first highly stable
 silicates with five hydrocarbon ligands
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              348
_journal_paper_doi               10.1039/b109816k
_journal_year                    2002
_chemical_formula_moiety         ' C16 H36 N, C25 H19 Si'
_chemical_formula_sum            'C41 H55 N Si'
_chemical_formula_weight         589.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.5485(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9938(2)
_cell_length_b                   19.2264(3)
_cell_length_c                   19.4424(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3502.16(10)
_computing_cell_refinement       'DENZO 1.11.0'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO 1.11.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56276
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+3.0971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                4809
_reflns_number_total             5828
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b109816k.txt
_cod_data_source_block           s2340a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7114104