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_4347511
_publ_section_title
;
 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 H32 F6 Li O4 P Si4, C H2 Cl2'
_chemical_formula_sum            'C13 H34 Cl2 F6 Li O4 P Si4'
_chemical_formula_weight         589.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1612(3)
_cell_length_b                   13.9035(5)
_cell_length_c                   19.6348(7)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.755
_cell_measurement_theta_min      2.539
_cell_volume                     2773.93(16)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31968
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.781
_diffrn_reflns_theta_min         2.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_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    1.412
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.488
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         9322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0240P)^2^+0.9570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                8220
_reflns_number_total             9322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00267_si_005.cif
_cod_data_source_block           kr206_0m
_cod_database_code               4347511
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.42(6) 0.58(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C13(H13A,H13B), C3(H3A,H3B), C4(H4A,H4B)
3.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              16405
_shelx_hkl_checksum              69344
_olex2_submission_special_instructions 'No special instructions were received'