Novel quadruple-stranded heterometallic Ln2Na complexes hosting sodium ions inside the cryptand-like cavity
Horniichuk, Oleksandr Ye.; Trush, Victor A.; Kariaka, Nataliia S.; Shishkina, Svitlana V.; Dyakonenko, Viktoriya V.; Severinovskaya, Olga V.; Gawryszewska, Paula; Domasevitch, Kostiantyn V.; Watras, Adam; Amirkhanov, Vladimir M.; New Journal of Chemistry 45 (2021) 22361–22368; doi:10.1039/D1NJ04353F

data_7061075
_publ_section_title
;
 Novel quadruple-stranded heterometallic Ln2Na complexes hosting sodium
 ions inside the cryptand-like cavity
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22361
_journal_page_last               22368
_journal_paper_doi               10.1039/D1NJ04353F
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H48 F24 N8 Na Nd2 O33 P8, C8 H20 N'
_chemical_formula_sum            'C44 H68 F24 N9 Na Nd2 O33 P8'
_chemical_formula_weight         2266.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8807(6)
_cell_length_b                   17.8807(6)
_cell_length_c                   16.2846(6)
_cell_measurement_reflns_used    7624
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.4870
_cell_measurement_theta_min      3.4520
_cell_volume                     5206.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -32.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283  -85.0000   -2.0000 40

  2 omega  -99.00  -59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283 -178.0000  120.0000 40

  3 omega  -68.00  -42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283 -178.0000  150.0000 26

  4 omega  -83.00  -57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283 -178.0000  -60.0000 26

  5 omega -103.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283    0.0000    0.0000 106

  6 omega  -52.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3283   77.0000  120.0000 93

  7 omega  -18.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.5783  -99.0000 -150.0000 84

  8 omega   -3.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.5783   77.0000  -30.0000 105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40536
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1584 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.086(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+10.7614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4061
_reflns_number_total             4579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04353f2.cif
_cod_data_source_block           k285
_cod_depositor_comments
'Adding full bibliography for 7061074--7061076.cif.'
_cod_original_cell_volume        5206.5(4)
_cod_database_code               7061075
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.580
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-O9 = C6-O5 = O6-C7
 1.45 with sigma of 0.002
 N3-C16
 1.5 with sigma of 0.02
 N3-C10
 1.55 with sigma of 0.02
 N3-C12 = N3-C14 = C14-C15
 1.54 with sigma of 0.02
 C12-C13
 1.51 with sigma of 0.02
 C16-C17
 1.49 with sigma of 0.02
 C10-C11
 1.56 with sigma of 0.02
 N3-C15
 2.56 with sigma of 0.04
 N3-C11
 2.62 with sigma of 0.04
 N3-C13
 2.58 with sigma of 0.04
 N3-C17
 2.52 with sigma of 0.04
 N3-C11 \\sim N3-C13 \\sim N3-C15 \\sim N3-C17
 with sigma of 0.04
 N3-C10 \\sim N3-C16 \\sim N3-C12 \\sim N3-C14
 with sigma of 0.02
 C10-C11 \\sim C12-C13 \\sim C14-C15 \\sim C16-C17
 with sigma of 0.02
 C10-C12 \\sim C12-C14 \\sim C14-C16 \\sim C16-C10
 with sigma of 0.04
 C11-C13 \\sim C13-C15 \\sim C15-C17
 with sigma of 0.08
3. Uiso/Uaniso restraints and constraints
P1 \\sim O5 \\sim C6: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
P1 \\sim O6 \\sim C7: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
P2 \\sim O9 \\sim C8: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
N3 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C14) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 N3, C10, C11, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Na1(0.25) N3(0.25) C10(0.25) H10A(0.25) H10B(0.25) C11(0.25)
 H11A(0.25) H11B(0.25) H11C(0.25) C12(0.25) H12A(0.25) H12B(0.25) C13(0.25)
 H13A(0.25) H13B(0.25) H13C(0.25) C14(0.25) H14A(0.25) H14B(0.25) C15(0.25)
 H15A(0.25) H15B(0.25) H15C(0.25) C16(0.25) H16A(0.25) H16B(0.25) C17(0.25)
 H17A(0.25) H17B(0.25) H17C(0.25)
6.a Riding coordinates:
 C6(H6A,H6B,H6C)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 98 electrons were 
found in a volume of 1508\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 5[H2O] per Formula Unit 
which account for 100 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8288
_shelx_fab_checksum              57564
_olex2_submission_special_instructions 'No special instructions were received'