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_2102494
_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         '4(C18 H16 O Si), C12 H10 N2'
_chemical_formula_sum            'C84 H74 N2 O4 Si4'
_chemical_formula_weight         1287.82
_chemical_name_systematic
;
Triphenylsilanol--1,2-bis(4-pyridyl)ethene (4/1)
;
_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
_cell_angle_alpha                64.5048(10)
_cell_angle_beta                 84.1339(10)
_cell_angle_gamma                79.7744(13)
_cell_formula_units_Z            1
_cell_length_a                   8.6418(2)
_cell_length_b                   14.1263(3)
_cell_length_c                   16.3149(4)
_cell_measurement_reflns_used    8105
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.65
_cell_volume                     1768.42(7)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23113
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.312
_refine_ls_extinction_coef       0.0085(14)
_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   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.5110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                6126
_reflns_number_total             8105
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na5012.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2019-10-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C18 H16 O Si), 0.5(C12 H10 N2)'
_cod_original_formula_sum        'C42 H37 N O2 Si2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     643.91
_cod_database_code               2102494