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_7133280
_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         'C12 H24 O6 Rb, C30 H50 Be Cl N2 Si2, C7 H8'
_chemical_formula_sum            'C52.5 H86 Be Cl N2 O6 Rb Si2'
_chemical_formula_weight         1027.34
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-16
_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                 103.361(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7051(3)
_cell_length_b                   21.1030(3)
_cell_length_c                   17.1977(3)
_cell_measurement_reflns_used    16096
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.7620
_cell_measurement_theta_min      4.1850
_cell_volume                     5898.57(18)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.416
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81592
_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    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         11800
_refine_ls_number_restraints     894
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+4.0777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9549
_reflns_number_total             11800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02725f2.cif
_cod_data_source_block           s22msh72-cpd-9
_cod_depositor_comments
'Adding full bibliography for 7133277--7133282.cif.'
_cod_original_formula_sum        'C52.50 H86 Be Cl N2 O6 Rb Si2'
_cod_database_code               7133280
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.685
_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
 C38-C37 = C38A-C37A = C40-C39 = C40A-C39A = C42-C41 = C42A-C41A = C32-C31 =
 C32A-C31A = C34-C33 = C34A-C33A = C36-C35 = C36A-C35A
 1.54 with sigma of 0.005
 O4-C37 \\sim O4A-C36A \\sim O4A-C37A \\sim O5-C38 \\sim O5A-C38A \\sim O5-C39
\\sim O5A-C39A \\sim O6-C40
 \\sim O6-C41 \\sim O6A-C40A \\sim O6A-C41A \\sim O1-C42 \\sim O1-C31 \\sim
O1A-C42A \\sim O1A-C31A \\sim O2-
 C32 \\sim O2A-C32A \\sim O2-C33 \\sim O2A-C33A \\sim O3-C34 \\sim O3-C35 \\sim
O3A-C34A \\sim O3A-C35A 
 O4-C36
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\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
C43A \\sim C47A \\sim C44A \\sim C48A \\sim C45A \\sim C49A \\sim C46A: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
O4A \\sim O4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
O3A \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
4. Others
 Fixed Sof: O1(0.55) O2(0.55) O3(0.55) O4(0.55) O5(0.55) O6(0.55) C31(0.55)
 H31A(0.55) H31B(0.55) C32(0.55) H32A(0.55) H32B(0.55) C33(0.55) H33A(0.55)
 H33B(0.55) C34(0.55) H34A(0.55) H34B(0.55) C35(0.55) H35A(0.55) H35B(0.55)
 C36(0.55) H36A(0.55) H36B(0.55) C37(0.55) H37A(0.55) H37B(0.55) C38(0.55)
 H38A(0.55) H38B(0.55) C39(0.55) H39A(0.55) H39B(0.55) C40(0.55) H40A(0.55)
 H40B(0.55) C41(0.55) H41A(0.55) H41B(0.55) C42(0.55) H42A(0.55) H42B(0.55)
 O1A(0.45) O2A(0.45) O3A(0.45) O4A(0.45) O5A(0.45) O6A(0.45) C31A(0.45)
 H31C(0.45) H31D(0.45) C32A(0.45) H32C(0.45) H32D(0.45) C33A(0.45) H33C(0.45)
 H33D(0.45) C34A(0.45) H34C(0.45) H34D(0.45) C35A(0.45) H35C(0.45) H35D(0.45)
 C36A(0.45) H36C(0.45) H36D(0.45) C37A(0.45) H37C(0.45) H37D(0.45) C38A(0.45)
 H38C(0.45) H38D(0.45) C39A(0.45) H39C(0.45) H39D(0.45) C40A(0.45) H40C(0.45)
 H40D(0.45) C41A(0.45) H41C(0.45) H41D(0.45) C42A(0.45) H42C(0.45) H42D(0.45)
 C43(0.67) H43A(0.67) H43B(0.67) H43C(0.67) C47(0.67) H47(0.67) C48(0.67)
 H48(0.67) C49(0.67) H49(0.67) C44(0.67) C45(0.67) H45(0.67) C46(0.67)
 H46(0.67) C43A(0.33) H43D(0.33) H43E(0.33) H43F(0.33) C44A(0.33) C45A(0.33)
 H45A(0.33) C46A(0.33) H46A(0.33) C47A(0.33) H47A(0.33) C48A(0.33) H48A(0.33)
 C49A(0.33) H49A(0.33)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C25(H25), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 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), C47(H47), C48(H48),
 C49(H49), C45(H45), C46(H46), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A),
 C49A(H49A)
5.d Fitted hexagon refined as free rotating group:
 C10(C5,C6,C7,C8,C9), C47(C48,C49,C44,C45,C46), C44A(C45A,C46A,C47A,C48A,C49A)
5.e 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), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79036
_shelx_hkl_checksum              18278
_shelx_fab_checksum              87987