NMR and X-ray Studies of Hydrogen Bonding for Amide-Containing Silanediols
Wilson, Sean O.; Tran, Ngon T.; Franz, Annaliese K.; Organometallics 31 (2012) 6715–6718; doi:10.1021/om300736n

data_4078999
_publ_section_title
;
 NMR and X-ray Studies of Hydrogen Bonding for Amide-Containing
 Silanediols
;
_journal_coden_ASTM              ORGND7
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6715
_journal_page_last               6718
_journal_paper_doi               10.1021/om300736n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         '2(C26 H33 N O3 Si), H2 O'
_chemical_formula_sum            'C26 H34 N O3.5 Si'
_chemical_formula_weight         444.63
_chemical_name_common
'2-[dihydroxy(mesityl)silyl]-N,N-diisopropylnaphthalene-1-carboxamide with water solvate'
_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
_audit_update_record
;
2012-05-29 # Formatted by publCIF
;
_cell_angle_alpha                96.38(2)
_cell_angle_beta                 100.07(2)
_cell_angle_gamma                110.888(19)
_cell_formula_units_Z            4
_cell_length_a                   10.944(3)
_cell_length_b                   14.793(5)
_cell_length_c                   16.344(3)
_cell_measurement_reflns_used    10483
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2390.4(12)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17867
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         10483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                6171
_reflns_number_total             10483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300736n_si_002.cif
_cod_data_source_block           a3
_cod_original_cell_volume        2390.3(10)
_cod_database_code               4078999