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_7715884
_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 H36 Mo8 N24 Na2 O20, 12.5[H2O], 8[H2O]'
_chemical_formula_sum            'C24 H77 Mo8 N24 Na2 O40.5'
_chemical_formula_weight         2163.59
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-16
_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            2
_cell_length_a                   18.2472(7)
_cell_length_b                   18.2472(7)
_cell_length_c                   10.4717(12)
_cell_measurement_reflns_used    2186
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.5850
_cell_measurement_theta_min      3.4270
_cell_volume                     3486.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -85.00 -48.00   0.50    2.13    --  -41.99-157.00  31.00   74
  2  \w   -123.00 -82.00   0.50    8.51    --  -96.00-119.00-173.00   82
  3  \w    -87.00 -21.00   0.50    8.51    --  -96.00  70.00  30.00  132
  4  \w   -163.00-133.00   0.50    8.51    --  -96.00-119.00-173.00   60
  5  \w    -19.00  36.00   0.50    2.13    --  -41.99  19.00 -90.00  110
  6  \w     80.00 108.00   0.50    2.13    --   41.99-157.00  31.00   56
  7  \w     53.00  79.00   0.50    2.13    --   41.99-157.00  31.00   52
  8  \w    -90.00 -48.00   0.50    8.51    --  -96.00 125.00  30.00   84
  9  \w    -51.00 -20.00   0.50    8.51    --  -96.00  45.00-180.00   62
 10  \w    -71.00 -41.00   0.50    8.51    --  -96.00  61.00   0.00   60
 11  \w     42.00  70.00   0.50    8.51    --  114.53 -61.00-150.00   56
 12  \w     42.00  71.00   0.50    8.51    --  114.53 -61.00-180.00   58
 13  \w     65.00  99.00   0.50    8.51    --  114.53 -77.00-180.00   68
 14  \w     45.00  71.00   0.50    8.51    --  114.53 -61.00  30.00   52
 15  \w     42.00  71.00   0.50    8.51    --  114.53 -61.00 150.00   58
 16  \w     42.00  67.00   0.50    8.51    --  114.53 -61.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0333413000
_diffrn_orient_matrix_UB_12      -0.0552032000
_diffrn_orient_matrix_UB_13      -0.0949033000
_diffrn_orient_matrix_UB_21      0.0404302000
_diffrn_orient_matrix_UB_22      -0.0630207000
_diffrn_orient_matrix_UB_23      0.0681071000
_diffrn_orient_matrix_UB_31      -0.0662071000
_diffrn_orient_matrix_UB_32      -0.0106958000
_diffrn_orient_matrix_UB_33      0.0893181000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        63.977
_diffrn_reflns_theta_max         63.977
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       prism
_exptl_crystal_F_000             2142
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0966P)^2^+2.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1281
_reflns_number_total             1545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00825a2.cif
_cod_data_source_block           exp_13141_auto
_cod_depositor_comments
'Adding full bibliography for 7715883--7715885.cif.'
_cod_original_cell_volume        3486.7(5)
_cod_original_formula_sum        'C24 H77 Mo8 N24 Na2 O40.50'
_cod_database_code               7715884
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Mo'
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.189
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.02
 Mo2-H7 \\sim Mo1_$1-H7
 with sigma of 0.02
3. Others
 Sof(H11)=Sof(N1)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(H9)=Sof(N3)=Sof(H3A)=Sof(H3B)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C10(H10)
4.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1614
_shelx_fab_checksum              16738
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.801