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_7125200
_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         'C13 H32 F3 Li O7 S Si4, C H2 Cl2'
_chemical_formula_sum            'C14 H34 Cl2 F3 Li O7 S Si4'
_chemical_formula_weight         593.67
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.6745(7)
_cell_length_b                   24.0048(11)
_cell_length_c                   32.5952(14)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.186
_cell_measurement_theta_min      2.52
_cell_volume                     11481.9(9)
_computing_molecular_graphics
;
%$getVar(olex2_reference_short)%
;
_computing_publication_material
;
%$getVar(olex2_reference_short)%
;
_computing_structure_refinement
;
%$getVar(refinement_reference_short)%
;
_computing_structure_solution
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0774
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            146908
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.327
_diffrn_reflns_theta_max         25.327
_diffrn_reflns_theta_min         2.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1750 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.9112. The \l/2 correction factor is 0.00150.'
_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    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.214
_refine_diff_density_max         2.079
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0500P)^2^+31.7070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8049
_reflns_number_total             10456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07520g2.cif
_cod_data_source_block           kr287pbca
_cod_database_code               7125200
_publ_section_exptl
;
Any special experimental details
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C23(H23A,H23B), C24(H24A,H24B), C12(H12A,
 H12B), C26(H26A,H26B), C25(H25A,H25B), C9(H9A,H9B), C14(H14A,H14B), C28(H28A,
 H28B)
2.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C17(H17A,H17B,H17C),
 C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C2(H2A,H2B,H2C), C18(H18A,H18B,H18C),
  C19(H19A,H19B,H19C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C),
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'