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_7055227
_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
;
C12 H24 K O6, C10 H8
;
_chemical_formula_sum            'C22 H32 K O6'
_chemical_formula_weight         431.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                98.5060(15)
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_cell_angle_gamma                113.2050(14)
_cell_formula_units_Z            2
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_cell_length_b                   9.1354(8)
_cell_length_c                   15.4095(14)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.46
_cell_volume                     1108.98(17)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11412
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.563
_diffrn_reflns_theta_min         1.342
_diffrn_source                   'fine-focus tube, MoK\a'
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.27
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_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0412P)^2^+0.3077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4238
_reflns_number_total             5873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02841h2.cif
_cod_data_source_block           940SF_0ms_a
_cod_depositor_comments
'Adding full bibliography for 7055227--7055237.cif.'
_cod_database_code               7055227
_shelxl_version_number           2014/6
_shelx_res_checksum              12878