Hydrogen-bonded adducts of triphenylsilanol with diamines: a finite ten-molecule aggregate, and chain, sheet and framework structures built from O—H···O, O—H···N and C—H···π(arene) hydrogen bonds
Turkington, David E.; Lough, Alan J.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section B 60 (2004) 238–248; doi:10.1107/S0108768104002344

data_2102495
_publ_section_title
;
 Hydrogen-bonded adducts of triphenylsilanol with diamines: a finite
 ten-molecule aggregate, and chain, sheet and framework structures
 built from O---H&#x00B7;&#x00B7;&#x00B7;O,
 O---H&#x00B7;&#x00B7;&#x00B7;N and
 C---H&#x00B7;&#x00B7;&#x00B7;\p(arene) hydrogen bonds
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              238
_journal_page_last               248
_journal_paper_doi               10.1107/S0108768104002344
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         '2(C18 H16 O Si), C6 H14 N2'
_chemical_formula_sum            'C42 H46 N2 O2 Si2'
_chemical_formula_weight         666.98
_chemical_name_systematic
;
Triphenylsilanol--N,N'-dimethylpiperazine (2/1)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.868(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6528(10)
_cell_length_b                   8.1361(4)
_cell_length_c                   16.7852(10)
_cell_measurement_reflns_used    3291
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.75
_cell_volume                     1769.00(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997) and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15411
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.398
_refine_ls_extinction_coef       0.011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0714P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                2276
_reflns_number_total             3291
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na5012.cif
_cod_data_source_block           III
_cod_depositor_comments
;

2019-10-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1769.00(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_moiety     'C18 H16 O Si, 0.5(C6 H14 N2)'
_cod_original_formula_sum        'C21 H23 N O Si'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     333.49
_cod_database_code               2102495