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_7133279
_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         'C30 H50 Be Cl N2 Si2, C20 H40 Na O10'
_chemical_formula_sum            'C50 H90 Be Cl N2 Na O10 Si2'
_chemical_formula_weight         1002.86
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-04
_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                 91.531(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1421(6)
_cell_length_b                   20.7692(7)
_cell_length_c                   18.2654(5)
_cell_measurement_reflns_used    6033
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.7340
_cell_measurement_theta_min      4.3030
_cell_volume                     5742.2(3)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.391
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76303
_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             2176
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         11441
_refine_ls_number_restraints     1280
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0862
_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^)+(0.1396P)^2^+3.9296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6919
_reflns_number_total             11441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02725f2.cif
_cod_data_source_block           s22msh65-cpd-7
_cod_depositor_comments
'Adding full bibliography for 7133277--7133282.cif.'
_cod_database_code               7133279
_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
 Na1-O2 \\sim Na1-O2A
 with sigma of 0.02
 O5-C37 \\sim O5A-C37A
 with sigma of 0.04
 Na1-O1 \\sim Na1-O1A
 with sigma of 0.02
 Na1-O3 \\sim Na1-O3A
 with sigma of 0.02
 Na1-O5 \\sim Na1-O5A
 with sigma of 0.02
 Na1-O4 \\sim Na1-O4A
 with sigma of 0.02
 O2-C32 \\sim O2A-C32A
 with sigma of 0.02
 O2-C33 \\sim O2A-C33A
 with sigma of 0.02
 C31-C40 \\sim C31A-C40A
 with sigma of 0.04
 O1-C31 \\sim O1A-C31A
 with sigma of 0.02
 O1-C40 \\sim O1A-C40A
 with sigma of 0.02
 O3-C36 \\sim O3A-C36A
 with sigma of 0.04
 O3-C35 \\sim O3A-C35A
 with sigma of 0.02
 O3-C34 \\sim O3A-C34A
 with sigma of 0.02
 O5-C38 \\sim O5A-C38A
 with sigma of 0.02
 O5-C39 \\sim O5A-C39A
 with sigma of 0.02
 C32-C31 \\sim C32A-C31A
 with sigma of 0.02
 O4-C37 \\sim O4A-C37A
 with sigma of 0.02
 O4-C38 \\sim O4A-C38A
 with sigma of 0.04
 O4-C36 \\sim O4A-C36A
 with sigma of 0.02
 C35-C34 \\sim C35A-C34A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 O3-C33 \\sim O3A-C33A
 with sigma of 0.04
 C40-C39 \\sim C40A-C39A
 with sigma of 0.02
 O5-C40 \\sim O5A-C40A
 with sigma of 0.04
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 O4-C35 \\sim O4A-C35A
 with sigma of 0.04
 Na1-C32 \\sim Na1-C32A
 with sigma of 0.04
 Na1-C31 \\sim Na1-C31A
 with sigma of 0.04
 Na1-C33 \\sim Na1-C33A
 with sigma of 0.04
 C37-C36 \\sim C37A-C36A
 with sigma of 0.04
 Na1-C35 \\sim Na1-C35A
 with sigma of 0.04
 Na1-C40 \\sim Na1-C40A
 with sigma of 0.04
 Na1-C37 \\sim Na1-C37A
 with sigma of 0.04
 Na1-C34 \\sim Na1-C34A
 with sigma of 0.04
 Na1-C36 \\sim Na1-C36A
 with sigma of 0.04
 Na1-C38 \\sim Na1-C38A
 with sigma of 0.04
 Na1-C39 \\sim Na1-C39A
 with sigma of 0.04
 O2-C31 \\sim O2A-C31A
 with sigma of 0.04
 O2-C34 \\sim O2A-C34A
 with sigma of 0.04
 C38-C39 \\sim C38A-C39A
 with sigma of 0.04
 O1-C32 \\sim O1A-C32A
 with sigma of 0.04
 O1-C39 \\sim O1A-C39A
 with sigma of 0.04
 O7-C43 \\sim O8-C44 \\sim O8-C45 \\sim O9-C47 \\sim O10-C48 \\sim O10-C49
\\sim O6-C50 \\sim O6-C41 \\sim O7-
 C42
 with sigma of 0.01
 C48-C47 \\sim C50-C49 \\sim C46-C45 \\sim C44-C43 \\sim C42-C41
 with sigma of 0.005
 O2A-C33A \\sim O2-C32 \\sim O2-C33 \\sim O3A-C34A \\sim O3A-C35A \\sim O3-C34
\\sim O3-C35 \\sim O4A-C36A
 \\sim O4A-C37A \\sim O5A-C38A \\sim O5A-C39A \\sim O5-C38 \\sim O5-C39 \\sim
O1A-C40A \\sim O1A-C31A \\sim O1-
 C40 \\sim O1-C31 \\sim O2A-C32A \\sim O4-C36 \\sim O4-C37
 with sigma of 0.005
 C42-O6 \\sim C42A-O6A
 with sigma of 0.04
 O7-C44 \\sim O7A-C44A
 with sigma of 0.04
 Na1-C42 \\sim Na1-C42A
 with sigma of 0.04
 Na1-C44 \\sim Na1-C44A
 with sigma of 0.04
 C47-O10 \\sim C47A-O10A
 with sigma of 0.04
 Na1-C46 \\sim Na1-C46A
 with sigma of 0.04
 O8-C43 \\sim O8A-C43A
 with sigma of 0.04
 C48-O9 \\sim C48A-O9A
 with sigma of 0.04
 C44-C45 \\sim C44A-C45A
 with sigma of 0.04
 Na1-O8 \\sim Na1-O8A
 with sigma of 0.02
 Na1-O7 \\sim Na1-O7A
 with sigma of 0.02
 Na1-O9 \\sim Na1-O9A
 with sigma of 0.02
 O8-C44 \\sim O8A-C44A
 with sigma of 0.02
 O8-C45 \\sim O8A-C45A
 with sigma of 0.02
 C42-O7 \\sim C42A-O7A
 with sigma of 0.02
 C42-C41 \\sim C42A-C41A
 with sigma of 0.02
 O7-C43 \\sim O7A-C43A
 with sigma of 0.02
 Na1-C47 \\sim Na1-C47A
 with sigma of 0.04
 Na1-C43 \\sim Na1-C43A
 with sigma of 0.04
 Na1-C45 \\sim Na1-C45A
 with sigma of 0.04
 O6-C41 \\sim O6A-C41A
 with sigma of 0.02
 O8-C46 \\sim O8A-C46A
 with sigma of 0.04
 O6-C50 \\sim O6A-C50A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.04
 C47-C48 \\sim C47A-C48A
 with sigma of 0.02
 C47-O9 \\sim C47A-O9A
 with sigma of 0.02
 O7-C41 \\sim O7A-C41A
 with sigma of 0.04
 C48-O10 \\sim C48A-O10A
 with sigma of 0.02
 O6-C49 \\sim O6A-C49A
 with sigma of 0.04
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 C47-C46 \\sim C47A-C46A
 with sigma of 0.04
 C48-C49 \\sim C48A-C49A
 with sigma of 0.04
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 C46-O9 \\sim C46A-O9A
 with sigma of 0.02
 C41-C50 \\sim C41A-C50A
 with sigma of 0.04
 C45-O9 \\sim C45A-O9A
 with sigma of 0.04
 C50-C49 \\sim C50A-C49A
 with sigma of 0.02
 C50-O10 \\sim C50A-O10A
 with sigma of 0.04
 C49-O10 \\sim C49A-O10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim O1 \\sim O3 \\sim O5 \\sim C32 \\sim O4 \\sim C31 \\sim C33 \\sim C35
\\sim C40 \\sim C37 \\sim C34 \\sim C36 \\sim C38 \\sim C39 \\sim O2A \\sim O1A
\\sim O3A \\sim O5A \\sim C32A \\sim O4A \\sim C31A \\sim C33A \\sim C35A \\sim
C40A \\sim C37A \\sim C34A \\sim C36A \\sim C38A \\sim C39A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
O8 \\sim C42 \\sim O7 \\sim O6 \\sim C47 \\sim C48 \\sim C44 \\sim C43 \\sim
C46 \\sim C41 \\sim C45 \\sim C50 \\sim O9 \\sim C49 \\sim O10 \\sim O8A \\sim
C42A \\sim O7A \\sim O6A \\sim C47A \\sim C48A \\sim C44A \\sim C43A \\sim C46A
\\sim C41A \\sim C45A \\sim C50A \\sim O9A \\sim C49A \\sim O10A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
Na2 \\sim Na1: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
4. Others
 Fixed Sof: Na1(0.67) O2(0.67) O1(0.67) O3(0.67) O5(0.67) C32(0.67) H32A(0.67)
 H32B(0.67) O4(0.67) C31(0.67) H31A(0.67) H31B(0.67) C33(0.67) H33A(0.67)
 H33B(0.67) C35(0.67) H35A(0.67) H35B(0.67) C40(0.67) H20(0.67) H24(0.67)
 C37(0.67) H37A(0.67) H37B(0.67) C34(0.67) H34A(0.67) H34B(0.67) C36(0.67)
 H36A(0.67) H36B(0.67) C38(0.67) H38A(0.67) H38B(0.67) C39(0.67) H1Y(0.67)
 H1Z(0.67) O8(0.67) C42(0.67) H42A(0.67) H42B(0.67) O7(0.67) O6(0.67) C47(0.67)
 H47A(0.67) H47B(0.67) C48(0.67) H48A(0.67) H48B(0.67) C44(0.67) H44A(0.67)
 H44B(0.67) C43(0.67) H43A(0.67) H43B(0.67) C46(0.67) H46A(0.67) H46B(0.67)
 C41(0.67) H41A(0.67) H41B(0.67) C45(0.67) H45A(0.67) H45B(0.67) C50(0.67)
 H50A(0.67) H50B(0.67) O9(0.67) C49(0.67) H49A(0.67) H49B(0.67) O10(0.67)
 O2A(0.33) O1A(0.33) O3A(0.33) O5A(0.33) C32A(0.33) H32C(0.33) H32D(0.33)
 O4A(0.33) C31A(0.33) H31C(0.33) H31D(0.33) C33A(0.33) H33C(0.33) H33D(0.33)
 C35A(0.33) H35C(0.33) H35D(0.33) C40A(0.33) H40A(0.33) H40B(0.33) C37A(0.33)
 H37C(0.33) H37D(0.33) C34A(0.33) H34C(0.33) H34D(0.33) C36A(0.33) H36C(0.33)
 H36D(0.33) C38A(0.33) H38C(0.33) H38D(0.33) C39A(0.33) H39A(0.33) H39B(0.33)
 O8A(0.33) C42A(0.33) H42C(0.33) H42D(0.33) O7A(0.33) O6A(0.33) C47A(0.33)
 H47C(0.33) H47D(0.33) C48A(0.33) H48C(0.33) H48D(0.33) C44A(0.33) H44C(0.33)
 H44D(0.33) C43A(0.33) H43C(0.33) H43D(0.33) C46A(0.33) H46C(0.33) H46D(0.33)
 C41A(0.33) H41C(0.33) H41D(0.33) C45A(0.33) H45C(0.33) H45D(0.33) C50A(0.33)
 H50C(0.33) H50D(0.33) O9A(0.33) C49A(0.33) H49C(0.33) H49D(0.33) O10A(0.33)
 Na2(0.33)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C28(H28), C14(H14), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C32(H32A,H32B), C31(H31A,H31B), C33(H33A,H33B),
 C35(H35A,H35B), C40(H20,H24), C37(H37A,H37B), C34(H34A,H34B), C36(H36A,H36B),
 C38(H38A,H38B), C39(H1Y,H1Z), C42(H42A,H42B), C47(H47A,H47B), C48(H48A,H48B),
 C44(H44A,H44B), C43(H43A,H43B), C46(H46A,H46B), C41(H41A,H41B), C45(H45A,H45B),
  C50(H50A,H50B), C49(H49A,H49B), C32A(H32C,H32D), C31A(H31C,H31D), C33A(H33C,
 H33D), C35A(H35C,H35D), C40A(H40A,H40B), C37A(H37C,H37D), C34A(H34C,H34D),
 C36A(H36C,H36D), C38A(H38C,H38D), C39A(H39A,H39B), C42A(H42C,H42D), C47A(H47C,
 H47D), C48A(H48C,H48D), C44A(H44C,H44D), C43A(H43C,H43D), C46A(H46C,H46D),
 C41A(H41C,H41D), C45A(H45C,H45D), C50A(H50C,H50D), C49A(H49C,H49D)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C23(H23), C9(H9), C8(H8), C22(H22)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C27(H27A,H27B,
 H27C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              45757
_shelx_hkl_checksum              17497