Synthesis and Hydrolysis‒Condensation Study of Water-Soluble Self-Assembled Pentacoordinate Polysilylamides
Sohail, Muhammad; Bassindale, Alan R.; Taylor, Peter G.; Korlyukov, Alexander A.; Arkhipov, Dmitry E.; Male, Louise; Coles, Simon J.; Hursthouse, Michael B.; Organometallics 32 (2013) 1721–; doi:10.1021/om301137b

data_4080371
_publ_section_title
;
 Synthesis and Hydrolysis--Condensation Study of Water-Soluble
 Self-Assembled Pentacoordinate Polysilylamides
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1721
_journal_paper_doi               10.1021/om301137b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'C15 H19 N2 O2 Si +, 0.75 H3 O +, 1.75 Cl -, 0.25 H2 O'
_chemical_formula_sum            'C15 H21.75 Cl1.75 N2 O3 Si'
_chemical_formula_weight         368.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.673(12)
_cell_angle_beta                 71.708(11)
_cell_angle_gamma                71.435(12)
_cell_formula_units_Z            2
_cell_length_a                   7.941(3)
_cell_length_b                   10.448(5)
_cell_length_c                   12.404(6)
_cell_measurement_reflns_used    2202
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      1.68
_cell_volume                     922.9(7)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type
'Crystal Logics diffractometer with Rigaku Saturn 724 CCD detector'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Diamond I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8082
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             387
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.7114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                2873
_reflns_number_total             3438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om301137b_si_002.cif
_cod_data_source_block           ssh0985
_cod_database_code               4080371