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_4347510
_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_sum            'C14 H32 F6 K O6 P Si2'
_chemical_formula_weight         536.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 119.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4027(13)
_cell_length_b                   12.3519(11)
_cell_length_c                   10.4989(9)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.25
_cell_volume                     1173.2(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.308
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.0362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3721
_reflns_number_total             4295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00267_si_003.cif
_cod_data_source_block           kr168p21
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347510
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              6669
_shelx_hkl_checksum              5838