Hybrid Disila-Crown Ethers as Hosts for Ammonium Cations: The O-Si-Si-O Linkage as an Acceptor for Hydrogen Bonding
Dankert, F.; Reuter, K.; Donsbach, C.; Von Hanisch, C.; Inorganics 6 (2018) 15–; doi:10.3390/inorganics6010015

data_1556580
_publ_section_title
;
 Hybrid Disila-Crown Ethers as Hosts for Ammonium Cations: The O-Si-Si-O
 Linkage as an Acceptor for Hydrogen Bonding
;
_journal_name_full               Inorganics
_journal_page_first              15
_journal_paper_doi               10.3390/inorganics6010015
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C14 H32 O6 Si2, F6 P, H4 N'
_chemical_formula_sum            'C14 H36 F6 N O6 P Si2'
_chemical_formula_weight         515.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 117.9120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4542(5)
_cell_length_b                   12.3869(6)
_cell_length_c                   10.6140(5)
_cell_measurement_reflns_used    34532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.568
_cell_measurement_theta_min      4.342
_cell_volume                     1214.57(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.284
_diffrn_reflns_theta_min         2.171
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.745200
_exptl_absorpt_correction_T_min  0.721100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.346
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.2084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4365
_reflns_number_total             4419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            compound3.cif
_cod_data_source_block           compound1
_cod_database_code               1556580
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.873
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H2 = N1-H1 = N1-H3 = N1-H4
 0.91 with sigma of 0.02
3. Others
 Sof(H5AA)=Sof(H5AB)=Sof(O3A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H7AA)=Sof(H7AB)=
 1-FVAR(1)
 Sof(H5BC)=Sof(H5BD)=Sof(H7BC)=Sof(H7BD)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(O3)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5AA,H5AB), C5(H5BC,H5BD), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C6A(H6AA,H6AB), C7(H7AA,H7AB),
 C7(H7BC,H7BD), C8(H8A,H8B), C6(H6A,H6B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;