The 1:1 adduct of triphenylsilanol and 4,4'-bipyridyl, and three pairwise-concomitant triclinic polymorphs of the 4:1 adduct having <i>Z</i>' = 0.5, 1 and 4
Bowes, Katharine F.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section B 59 (2003) 277–286; doi:10.1107/S0108768103005196

data_2103877
_publ_section_title
;
 The 1:1 adduct of triphenylsilanol and 4,4'-bipyridyl, and three
 pairwise-concomitant triclinic polymorphs of the 4:1 adduct having
 <i>Z</i>' = 0.5, 1 and 4
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              277
_journal_page_last               286
_journal_paper_doi               10.1107/S0108768103005196
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         '4(C18 H16 O Si), C10 H8 N2'
_chemical_formula_sum            'C82 H72 N2 O4 Si4'
_chemical_formula_weight         1261.78
_chemical_name_systematic
;
Triphenylsilanol--4,4'-bipyridyl (4/1), polymorph with Z' = 0.5
;
_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                99.65(3)
_cell_angle_beta                 93.21(3)
_cell_angle_gamma                99.57(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2128(18)
_cell_length_b                   10.244(2)
_cell_length_c                   19.036(4)
_cell_measurement_reflns_used    10145
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     1740.0(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, 2002)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997a) and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22073
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.256
_refine_ls_extinction_coef       0.015(4)
_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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7927
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0798P)^2^+0.4962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1831
_reflns_number_gt                4784
_reflns_number_total             7927
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0147.cif
_cod_data_source_block           II
_cod_database_code               2103877
_cod_database_fobs_code          2103877