Synthesis and coordination ability of a partially silicon based crown ether.
Reuter, Kirsten; Thiele, Günther; Hafner, Thomas; Uhlig, Frank; von Hänisch, Carsten; Chemical communications (Cambridge, England) 52 (2016) 13265–13268; doi:10.1039/c6cc07520g

data_7125199
_publ_section_title
;
 Synthesis and coordination ability of a partially silicon based crown
 ether.
;
_journal_issue                   90
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13265
_journal_page_last               13268
_journal_paper_doi               10.1039/c6cc07520g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C9 H16 F3 Li O7 S'
_chemical_formula_sum            'C9 H16 F3 Li O7 S'
_chemical_formula_weight         332.22
_chemical_name_systematic        '[Li([12]crown-4)OTf]'
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-17 deposited with the CCDC.
2016-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.427(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0179(3)
_cell_length_b                   13.5605(6)
_cell_length_c                   14.8661(7)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.76
_cell_volume                     1405.86(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       rotational
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45249
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.476
_diffrn_reflns_theta_min         2.758
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0781 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.9733.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.543
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.201
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0308P)^2^+0.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3247
_reflns_number_total             3538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07520g2.cif
_cod_data_source_block           kr234b_0m
_cod_database_code               7125199
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.02 and sigma for terminal atoms of 0.05
: with sigma of 0.02 and sigma for terminal atoms of 0.05
3. Others
 Sof(O1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(O2B)=
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(O3B)=Sof(C4B)=
 Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(O4B)=Sof(C6B)=Sof(H6BA)=
 Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=1-FVAR(1)
 Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O2A)=
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(O3A)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O4A)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C8A(H8AA,H8AB), C1B(H1BA,H1BB), C8B(H8BA,H8BB), C3A(H3AA,
 H3AB), C2A(H2AA,H2AB), C3B(H3BA,H3BB), C2B(H2BA,H2BB), C4A(H4AA,H4AB),
 C5A(H5AA,H5AB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6A(H6AA,H6AB), C7A(H7AA,H7AB),
  C6B(H6BA,H6BB), C7B(H7BA,H7BB)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'