Isolation of gravimetrically quantifiable alkali metal arenides using 18-crown-6
Castillo, Maximiliano; Metta-Magaña, Alejandro J.; Fortier, Skye; New J. Chem. 40 (2016) 1923–; doi:10.1039/C5NJ02841H

data_7055236
_publ_section_title
;
 Isolation of gravimetrically quantifiable alkali metal arenides using
 18-crown-6
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1923
_journal_paper_doi               10.1039/C5NJ02841H
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C20 H40 Li1 O8, C20 H12'
_chemical_formula_sum            'C40 H52 K O8'
_chemical_formula_weight         699.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.461(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5120(18)
_cell_length_b                   18.3856(19)
_cell_length_c                   23.115(2)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.855
_cell_measurement_theta_min      2.215
_cell_volume                     7361.3(12)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58331
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_min         1.176
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       Platty
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.072
_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     903
_refine_ls_number_reflns         18221
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0681P)^2^+8.2240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11429
_reflns_number_total             18221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02841h2.cif
_cod_data_source_block           1025SF1_0mS
_cod_depositor_comments
'Adding full bibliography for 7055227--7055237.cif.'
_cod_original_cell_volume        7361.5(13)
_cod_database_code               7055236
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014/6
_shelx_res_checksum              7865