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_2102021
_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, C6 H12 N4'
_chemical_formula_sum            'C30 H34 N4 O3 Si2'
_chemical_formula_weight         554.79
_chemical_name_systematic
;
1,1,3,3-Tetraphenyldisiloxane-1,3-diol--hexamethylenetetramine (1/1)
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.386(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1555(9)
_cell_length_b                   8.4622(10)
_cell_length_c                   21.8427(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      14.20
_cell_measurement_theta_min      9.35
_cell_volume                     2961.4(4)
_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  .012
_diffrn_reflns_av_sigmaI/netI    .0703
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6651
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        6.9
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .157
_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    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .20
_refine_diff_density_max         .259
_refine_diff_density_min         -.238
_refine_ls_extinction_coef       .0027(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   .946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6436
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      .950
_refine_ls_R_factor_all          .1075
_refine_ls_R_factor_gt           .0443
_refine_ls_shift/su_max          .048
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1156
_reflns_number_gt                3416
_reflns_number_total             6436
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cf0008.cif
_cod_data_source_block           sila3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2102021
_cod_database_fobs_code          2102021