Oligosiloxanediols as building blocks for supramolecular chemistry: hydrogen-bonded adducts with amines form supramolecular structures in zero, one and two dimensions
O'Leary, Brian; Spalding, Trevor R.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section B 56 (2000) 273–286; doi:10.1107/S0108768199013051

data_2102025
_publ_section_title
;
 Oligosiloxanediols as building blocks for supramolecular chemistry:
 hydrogen-bonded adducts with amines form supramolecular structures in
 zero, one and two dimensions
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              273
_journal_page_last               286
_journal_paper_doi               10.1107/S0108768199013051
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C24 H22 O3 Si2, C4 H4 N2'
_chemical_formula_sum            'C28 H26 N2 O3 Si2'
_chemical_formula_weight         494.69
_chemical_name_systematic
;
1,1,3,3-Tetraphenyldisiloxane-1,3-diol--pyrimidine (1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                76.000(7)
_cell_angle_beta                 84.438(9)
_cell_angle_gamma                86.372(12)
_cell_formula_units_Z            1
_cell_length_a                   6.4358(5)
_cell_length_b                   10.2497(12)
_cell_length_c                   10.4056(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      17.00
_cell_measurement_theta_min      9.50
_cell_volume                     662.32(11)
_computing_cell_refinement
'SET4 & CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD-4-PC Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'DATRD2 in NRCVAX96 (Gabe et al., 1989)'
_computing_molecular_graphics
'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998)'
_computing_publication_material
'NRCVAX96, SHELXL97  and WordPerfect macro PREP8 (Ferguson, 1998)'
_computing_structure_refinement  'NRCVAX96 and SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_av_sigmaI/netI    .0158
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2876
_diffrn_reflns_theta_full        26.91
_diffrn_reflns_theta_max         26.91
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        'no decay, variation 0.6'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .165
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             260
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .36
_refine_diff_density_max         .319
_refine_diff_density_min         -.388
_refine_ls_extinction_coef       .028(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          .0521
_refine_ls_R_factor_gt           .0423
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.1328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2\s(I)
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_cod_data_source_block           sila7
_cod_database_code               2102025
_cod_database_fobs_code          2102025