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_7133278
_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         'C18 H36 K O9, C30 H50 Be Cl N2 Si2'
_chemical_formula_sum            'C48 H86 Be Cl K N2 O9 Si2'
_chemical_formula_weight         974.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-19 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.53220(10)
_cell_length_b                   21.8852(2)
_cell_length_c                   24.2440(2)
_cell_measurement_reflns_used    25645
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.5180
_cell_measurement_theta_min      4.1540
_cell_volume                     5584.43(9)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75169
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.720
_diffrn_reflns_theta_min         3.649
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81170
_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    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         11053
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0587P)^2^+1.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9789
_reflns_number_total             11053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02725f2.cif
_cod_data_source_block           s22msh61-cpd-8
_cod_depositor_comments
'Adding full bibliography for 7133277--7133282.cif.'
_cod_database_code               7133278
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.600
_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
 O3A-C35A \\sim O3-C34 \\sim O3-C35 \\sim O4A-C36A \\sim O4A-C37A \\sim O4-C36
\\sim O4-C37 \\sim O5A-C38A
 \\sim O5A-C39A \\sim O5-C38 \\sim O5-C39 \\sim O6A-C40A \\sim O6-C41 \\sim
O6-C40 \\sim O6A-C41A \\sim O1A-
 C42A \\sim O1A-C31A \\sim O1-C42 \\sim O1-C31 \\sim O10-C32A \\sim O10-C33A
\\sim O2-C32 \\sim O2-C33 
 O3A-C34A
 with sigma of 0.005
 C36A-C35A \\sim C36-C35 \\sim C38A-C37A \\sim C38-C37 \\sim C40A-C39A \\sim
C40-C39 \\sim C42A-C41A 
 C42-C41 \\sim C32A-C31A \\sim C32-C31 \\sim C34A-C33A \\sim C34-C33
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C31A \\sim C32A \\sim C33A \\sim C34A
\\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A
\\sim C42A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
4. Others
 Fixed Sof: O1(0.65) O2(0.65) O3(0.65) O4(0.65) O5(0.65) O6(0.65) C31(0.65)
 H31A(0.65) H31B(0.65) C32(0.65) H32A(0.65) H32B(0.65) C33(0.65) H33A(0.65)
 H33B(0.65) C34(0.65) H34A(0.65) H34B(0.65) C35(0.65) H35A(0.65) H35B(0.65)
 C36(0.65) H36A(0.65) H36B(0.65) C37(0.65) H37A(0.65) H37B(0.65) C38(0.65)
 H38A(0.65) H38B(0.65) C39(0.65) H39A(0.65) H39B(0.65) C40(0.65) H40A(0.65)
 H40B(0.65) C41(0.65) H41A(0.65) H41B(0.65) C42(0.65) H42A(0.65) H42B(0.65)
 O1A(0.35) O3A(0.35) O4A(0.35) O5A(0.35) O6A(0.35) O10(0.35) C31A(0.35)
 H31C(0.35) H31D(0.35) C32A(0.35) H32C(0.35) H32D(0.35) C33A(0.35) H33C(0.35)
 H33D(0.35) C34A(0.35) H34C(0.35) H34D(0.35) C35A(0.35) H35C(0.35) H35D(0.35)
 C36A(0.35) H36C(0.35) H36D(0.35) C37A(0.35) H37C(0.35) H37D(0.35) C38A(0.35)
 H38C(0.35) H38D(0.35) C39A(0.35) H39C(0.35) H39D(0.35) C40A(0.35) H40C(0.35)
 H40D(0.35) C41A(0.35) H41C(0.35) H41D(0.35) C42A(0.35) H42C(0.35) H42D(0.35)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C25(H25), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C31A(H31C,
 H31D), C32A(H32C,H32D), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D), C37A(H37C,H37D), C38A(H38C,H38D), C39A(H39C,H39D), C40A(H40C,
 H40D), C41A(H41C,H41D), C42A(H42C,H42D), C1(H1A,H1B), C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C21(H21), C22(H22), C23(H23)
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), C17(H17A,H17B,H17C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              81052
_shelx_hkl_checksum              47151
_olex2_submission_special_instructions 'No special instructions were received'