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_1556581
_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
'C18 H32 O6 Si2, H4 N, 1.28(C0.78 H1.56 Cl1.56), F6 P'
_chemical_formula_sum            'C19 H38 Cl2 F6 N O6 P Si2'
_chemical_formula_weight         648.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 104.950(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9582(7)
_cell_length_b                   12.6454(6)
_cell_length_c                   16.3325(8)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.30
_cell_volume                     2984.8(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.785
_diffrn_reflns_theta_min         2.140
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 2451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6355
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0615P)^2^+7.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5664
_reflns_number_total             6355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            compound4.cif
_cod_data_source_block           compound4
_cod_database_code               1556581
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(14)
 -0.01(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,
  H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H2 = N1-H3 = N1-H4 = N1-H1
 0.91 with sigma of 0.02
 Si2A-Si1A \\sim Si1-Si2
 with sigma of 0.02
 H1-H3 \\sim H1-H2 \\sim H1-H4 \\sim H3-H3 \\sim H3-H4 \\sim H2-H4
 with sigma of 0.02
 Cl13-C20 \\sim Cl14-C20 \\sim Cl1-C19 \\sim Cl2-C19 \\sim Cl1-C19A \\sim
Cl2A-C19A
 with sigma of 0.02
 Cl14-Cl13 \\sim Cl1-Cl2 \\sim Cl1-Cl2A
 with sigma of 0.02
 Si2-C4 \\sim Si2-C3 \\sim Si2A-C3A \\sim Si2A-C4A \\sim Si1-C1 \\sim Si1-C2
\\sim Si1A-C1A \\sim Si1A-C2A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A \\sim C2-C1 \\sim C2A-C1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl2A \\sim Cl1 \\sim C19 \\sim Cl13 \\sim Cl14 \\sim C20 \\sim C19A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Si2 \\sim Si1 \\sim O6 \\sim C2 \\sim C4 \\sim C1 \\sim C3 \\sim Si1A \\sim
Si2A \\sim O6A \\sim C3A \\sim C4A \\sim C1A \\sim C2A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(Cl14) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(Cl13) \\sim Ueq, Uanis(Cl1) \\sim Ueq,
Uanis(C19A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Si2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6A)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(Si2A) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C4A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(Si1) \\sim Ueq, Uanis(Si1A)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4) = Uanis(C4A)
5. Rigid body (RIGU) restrains
 Cl2, Cl2A, Cl1, C19, Cl13, Cl14, C20, C19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si2, Si1, O6, C2, C4, C1, C3, Si1A, Si2A, O6A, C3A, C4A, C1A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H5BC)=Sof(H5BD)=Sof(Cl13)=Sof(Cl14)=Sof(Si1A)=Sof(Si2A)=Sof(O6A)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=0.5*(1-FVAR(2))
 Sof(Cl2A)=Sof(C19A)=Sof(H19C)=Sof(H19D)=0.4*FVAR(2)
 Sof(Cl2)=Sof(C19)=Sof(H19A)=Sof(H19B)=0.6*FVAR(2)
 Sof(H5AA)=Sof(H5AB)=Sof(Cl1)=Sof(Si2)=Sof(Si1)=Sof(O6)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=Sof(H2C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(H1C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C7(H7A,H7B), C18(H18A,H18B), C16(H16A,H16B), C6(H6A,H6B),
 C8(H8A,H8B), C17(H17A,H17B), C5(H5AA,H5AB), C5(H5BC,H5BD), C19(H19A,H19B),
 C19A(H19C,H19D), C20(H20A,H20B)
7.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C11(H11), C10(H10)
7.c Disordered Me refined with riding coordinates:
 C2A(H2AA,H2AB,H2AC,H2AD,H2AE,H2AF)
7.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C3A(H3AA,
 H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              4525
_shelx_hkl_checksum              95572