Stable Alkali-Metal Complexes of Hybrid Disila-Crown Ethers.
Reuter, Kirsten; Buchner, Magnus R.; Thiele, Günther; von Hänisch, Carsten; Inorganic chemistry 55 (2016) 4441–4447; doi:10.1021/acs.inorgchem.6b00267

data_4347513
_publ_section_title
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 Stable Alkali-Metal Complexes of Hybrid Disila-Crown Ethers.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4441
_journal_page_last               4447
_journal_paper_doi               10.1021/acs.inorgchem.6b00267
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C12 H28 Cl Na O9 Si2, C6 H6'
_chemical_formula_sum            'C18 H34 Cl Na O9 Si2'
_chemical_formula_weight         509.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                91.291(2)
_cell_angle_beta                 92.820(2)
_cell_angle_gamma                97.259(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8536(5)
_cell_length_b                   9.9654(5)
_cell_length_c                   13.0638(6)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.152
_cell_measurement_theta_min      2.540
_cell_volume                     1270.44(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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker QUEST D8'
_diffrn_measurement_method       rotational
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33119
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.183
_diffrn_reflns_theta_min         2.540
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.305
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5632
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_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0564P)^2^+1.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4931
_reflns_number_total             5632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00267_si_002.cif
_cod_data_source_block           kr126_p-1
_cod_database_code               4347513
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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), C8(H8A,H8B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,H12B),
 C6(H6A,H6B), C9(H9A,H9B), C5(H5A,H5B)
2.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C17(H17), C15(H15), C14(H14), C16(H16)
;
_shelx_res_checksum              92524
_shelx_hkl_checksum              76885
_olex2_submission_special_instructions 'No special instructions were received'