Alkali metal reduction of crown ether encapsulated alkali metal cations.
Pearce, Kyle G.; Neale, Samuel E.; Mahon, Mary F.; McMullin, Claire L.; Hill, Michael S.; Chemical communications (Cambridge, England) 60 (2024) 8391–8394; doi:10.1039/d4cc02725f

data_7133282
_publ_section_title
;
 Alkali metal reduction of crown ether encapsulated alkali metal cations.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8391
_journal_page_last               8394
_journal_paper_doi               10.1039/d4cc02725f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C16 H32 K O8, C30 H50 Be Cl N2 Si2'
_chemical_formula_sum            'C46 H82 Be Cl K N2 O8 Si2'
_chemical_formula_weight         930.87
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-19 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.633(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9011(3)
_cell_length_b                   19.7649(3)
_cell_length_c                   18.0278(3)
_cell_measurement_reflns_used    14048
_cell_measurement_temperature    149.9(7)
_cell_measurement_theta_max      28.6250
_cell_measurement_theta_min      3.3770
_cell_volume                     5298.86(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61223
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.128
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.268
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 7095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.094(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         26216
_refine_ls_number_restraints     547
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0783P)^2^+1.2135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                19042
_reflns_number_total             26216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02725f2.cif
_cod_data_source_block           e22msh16-cpd-11
_cod_depositor_comments
'Adding full bibliography for 7133277--7133282.cif.'
_cod_original_cell_volume        5298.85(16)
_cod_database_code               7133282
_shelxl_version_number           2014-3
_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. Restrained distances
 O12A-C79A \\sim O12A-C80A \\sim O9A-C81A \\sim O9A-C74A \\sim O9-C81 \\sim
O9-C74 \\sim O10-C75 \\sim O10-
 C76 \\sim O10A-C76A \\sim O10A-C75A \\sim O12-C79 \\sim O12-C80 \\sim O11-C78
\\sim O11-C77 \\sim O11A-
 C77A \\sim O11A-C78A
 with sigma of 0.005
 C77-C76 \\sim C79A-C78A \\sim C79-C78 \\sim C81A-C80A \\sim C81-C80 \\sim
C75A-C74A \\sim C75-C74 
 C77A-C76A
 with sigma of 0.005
 O12-O10 \\sim O11-O9
 with sigma of 0.04
 O12A-O10A \\sim O11A-O9A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.015 and
sigma for terminal atoms of 0.01 within 2A
O9 \\sim O10 \\sim O11 \\sim O12 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim
C78 \\sim C79 \\sim C80 \\sim C81 \\sim O9A \\sim O10A \\sim O11A \\sim O12A
\\sim C74A \\sim C75A \\sim C76A \\sim C77A \\sim C78A \\sim C79A \\sim C80A
\\sim C81A: within 2A with sigma of 0.015 and sigma for terminal atoms of 0.01
within 2A
4. Others
 Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C74A)=Sof(H74C)=Sof(H74D)=
 Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)=Sof(C77A)=
 Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=Sof(C79A)=Sof(H79C)=
 Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=Sof(C81A)=Sof(H81C)=Sof(H81D)=1-FVAR(1)
 Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=
 Sof(H80B)=Sof(C81)=Sof(H81A)=Sof(H81B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26), C020(H020), C41(H41), C52(H52),
 C55(H55)
5.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
  C72(H72A,H72B), C73(H73A,H73B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,
 H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
 C89(H89A,H89B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C74A(H74C,
 H74D), C75A(H75C,H75D), C76A(H76C,H76D), C77A(H77C,H77D), C78A(H78C,H78D),
 C79A(H79C,H79D), C80A(H80C,H80D), C81A(H81C,H81D), C1(H1A,H1B), C2(H2A,H2B),
 C31(H31A,H31B), C32(H32A,H32B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C37(H37), C38(H38),
 C39(H39), C48(H48), C49(H49), C50(H50)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C2Z(H2ZA,H2ZB,H2ZC), C025(H02A,H02B,H02C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              61891
_shelx_hkl_checksum              41421