Crown ether-like octanuclear molybdenum(V) clusters for cation binding and gas adsorption.
Dai, Ru-Dan; Xie, Zhen-Lang; Liu, Cheng; Xin, Dong; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8980–8987; doi:10.1039/d4dt00825a

data_7715885
_publ_section_title
;
 Crown ether-like octanuclear molybdenum(V) clusters for cation binding
 and gas adsorption.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8980
_journal_page_last               8987
_journal_paper_doi               10.1039/d4dt00825a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H32 Mo16 N24 Na2 O49'
_chemical_formula_sum            'C24 H29 Mo16 N23 Na2 O49'
_chemical_formula_weight         3004.72
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.8779(2)
_cell_length_b                   32.8779(2)
_cell_length_c                   20.6940(2)
_cell_measurement_reflns_used    18498
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.9900
_cell_measurement_theta_min      3.4130
_cell_volume                     22369.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -38.00  28.00   1.00    5.00    --  -40.50  37.00 -60.00   66
  2  \w     37.00  92.00   1.00    5.00    --   43.29-125.00 150.00   55
  3  \w    110.00 144.00   1.00   11.00    --   95.91  77.00-150.00   34
  4  \w    116.00 164.00   1.00   11.00    --   95.91 125.00 -60.00   48
  5  \w    103.00 148.00   1.00   11.00    --   95.91  77.00 -60.00   45
  6  \w     16.00 102.00   1.00   11.00    --   95.91 -94.00  30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0317449000
_diffrn_orient_matrix_UB_12      -0.0297423000
_diffrn_orient_matrix_UB_13      0.0277007000
_diffrn_orient_matrix_UB_21      -0.0022240000
_diffrn_orient_matrix_UB_22      0.0218770000
_diffrn_orient_matrix_UB_23      0.0657021000
_diffrn_orient_matrix_UB_31      -0.0343949000
_diffrn_orient_matrix_UB_32      -0.0288824000
_diffrn_orient_matrix_UB_33      0.0212818000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46232
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        63.995
_diffrn_reflns_theta_max         63.995
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             11360
_refine_diff_density_max         1.792
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.451(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         18230
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0835P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                16038
_reflns_number_total             18230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00825a2.cif
_cod_data_source_block           exp_17703_auto
_cod_depositor_comments
'Adding full bibliography for 7715883--7715885.cif.'
_cod_database_code               7715885
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.549(17)
 0.451(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
Na1 \\sim H03V: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Na21 \\sim Na1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O00V \\sim O015 \\sim O016 \\sim O00S \\sim O00J \\sim Na3: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C02Z: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
Uanis(C03Z) \\sim Ueq, Uanis(C03V) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O00V) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq, Uanis(C02G) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N01O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na21) \\sim Ueq, Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C02A) \\sim Ueq, Uanis(C03J) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N01H) \\sim Ueq, Uanis(N029) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O00U) \\sim Ueq, Uanis(C03L) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N02H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N01I) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(H03I)=Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(Na1)=1-FVAR(1)
 Sof(H02T)=Sof(N17)=Sof(H17A)=Sof(H17B)=Sof(Na21)=FVAR(1)
 Fixed Sof: H02I(0.5) H03G(0.5) N11(0.5) H11A(0.5) H11B(0.5) N13(0.5)
 H13A(0.5) H13B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C027(H027), C02A(H02A), C02B(H02B), C02F(H02F), C02I(H02I), C02T(H02T),
 C02Z(H02Z), C032(H032), C034(H034), C035(H035), C039(H039), C03D(H03G),
 C03E(H03H), C03F(H03I), C03G(H03J), C03L(H03L), C03M(H03M), C03V(H03V)
5.b X=CH2 refined with riding coordinates:
 N01Z(H01A,H01B), N02H(H02C,H02D), N02L(H02E,H02G), N031(H03A,H03B), N036(H03C,
 H03D), N03C(H03E,H03F), N1(H1A,H1B), N17(H17A,H17B), N11(H11A,H11B), N13(H13A,
 H13B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90078
_shelx_fab_checksum              31689
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.463
_oxdiff_exptl_absorpt_empirical_full_min 0.720