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_7715883
_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         'C12 H16 K4 Mo8 N12 O26.875, 7[H2O]'
_chemical_formula_sum            'C24 H33.82 K8 Mo16 N24 O53.85'
_chemical_formula_weight         3367.93
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.36410(10)
_cell_length_b                   24.4988(2)
_cell_length_c                   25.6724(2)
_cell_measurement_reflns_used    41013
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3760
_cell_measurement_theta_min      3.2070
_cell_volume                     9602.98(13)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.952
_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    -97.00 -70.00   0.50    4.20    --  -41.99 139.00 -60.00   54
  2  \w   -115.00 -74.00   0.50    4.20    --  -41.99-131.00  54.00   82
  3  \w   -101.00 -75.00   0.50    4.20    --  -41.99-139.00-120.00   52
  4  \w     49.00 104.00   0.50    4.20    --   41.99-139.00-120.00  110
  5  \w   -132.00 -62.00   0.50   16.00    --  -96.00-139.00-120.00  140
  6  \w    -84.00 -59.00   0.50   16.00    --  -96.00 131.00 124.00   50
  7  \w     48.00  83.00   0.50   16.00    --  114.53-131.00  54.00   70
  8  \w     94.00 120.00   0.50   16.00    --  114.53 139.00 -60.00   52
  9  \w     50.00 126.00   0.50   16.00    --  114.53-139.00-120.00  152
 10  \w     94.00 121.00   0.50   16.00    --  114.53-131.00  54.00   54
 11  \w    -36.00  29.00   0.50    4.20    --  -41.99  38.00  60.00  130
 12  \w    -27.00  40.00   0.50    4.20    --  -41.99  19.00 -30.00  134
 13  \w    -24.00   1.00   0.50    4.20    --  -41.99  19.00 120.00   50
 14  \w     43.00  68.00   0.50    4.20    --   41.99-131.00  54.00   50
 15  \w   -172.00 -79.00   0.50   16.00    --  -96.00 -45.00  90.00  186
 16  \w    -48.00 -19.00   0.50   16.00    --  -96.00  45.00 -60.00   58
 17  \w    -51.00 -20.00   0.50   16.00    --  -96.00  45.00-120.00   62
 18  \w    -55.00 -29.00   0.50   16.00    --  -96.00  61.00 -30.00   52
 19  \w    -68.00 -23.00   0.50   16.00    --  -96.00 125.00-150.00   90
 20  \w    -51.00 -26.00   0.50   16.00    --  -96.00  45.00 -30.00   50
 21  \w     42.00  68.00   0.50   16.00    --  114.53 -61.00-120.00   52
 22  \w     93.00 169.00   0.50   16.00    --  114.53 125.00-180.00  152
 23  \w     42.00  70.00   0.50   16.00    --  114.53 -61.00  90.00   56
 24  \w     43.00  68.00   0.50   16.00    --  114.53 -61.00-180.00   50
 25  \w     95.00 178.00   0.50   16.00    --  114.53 125.00  90.00  166
 26  \w     77.00 103.00   0.50   16.00    --  114.53 -77.00-150.00   52
 27  \w     69.00  94.00   0.50   16.00    --  114.53 -95.00  60.00   50
 28  \w     48.00 116.00   0.50   16.00    --  114.53-125.00 -90.00  136
 29  \w     59.00  84.00   0.50   16.00    --  114.53 -77.00-180.00   50
 30  \w     46.00  71.00   0.50   16.00    --  114.53 -77.00-150.00   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      0.0820282000
_diffrn_orient_matrix_UB_12      0.0005398000
_diffrn_orient_matrix_UB_13      0.0404348000
_diffrn_orient_matrix_UB_21      -0.0023562000
_diffrn_orient_matrix_UB_22      0.0628494000
_diffrn_orient_matrix_UB_23      0.0009757000
_diffrn_orient_matrix_UB_31      -0.0586763000
_diffrn_orient_matrix_UB_32      -0.0018046000
_diffrn_orient_matrix_UB_33      0.0448626000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65412
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.776
_diffrn_reflns_theta_min         2.500
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34223
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_description       block
_exptl_crystal_F_000             6402
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.433
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         19500
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0562P)^2^+105.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17701
_reflns_number_total             19500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00825a2.cif
_cod_data_source_block           exp_13205_auto
_cod_depositor_comments
'Adding full bibliography for 7715883--7715885.cif.'
_cod_database_code               7715883
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Mo K'
_shelx_estimated_absorpt_t_max   0.234
_shelx_estimated_absorpt_t_min   0.149
_reflns_odcompleteness_completeness 99.73
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 K5-H5A \\sim K5-H5B
 with sigma of 0.02
 K15-O01M \\sim K7-O01M
 with sigma of 0.02
3. Rigid bond restraints
 K4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O7 \\sim O3 \\sim O5 \\sim O9: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
O5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
K7 \\sim K15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O01O \\sim K4B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
K4A \\sim K4B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O4 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O5A \\sim O18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
K5 \\sim K19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(K4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O5A, K6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O5A, O18, K6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O01M, K15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 K7, O01M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 K4A, K4B, O01O
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O4, O6, K6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O01W, K19, K5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(K1)=Sof(O4)=1-FVAR(1)
 Sof(K2)=Sof(O3)=Sof(O6)=Sof(O18)=FVAR(1)
 Sof(K4B)=1-FVAR(2)
 Sof(K4A)=Sof(O5A)=Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(2)
 Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(3)
 Fixed Sof: K3(0.5) O2(0.5) K5(0.75) K7(0.8) K6(0.5) K15(0.2) K19(0.25)
7.a Riding coordinates:
 O5(H5A,H5B), O7(H7A,H7B)
7.b Aromatic/amide H refined with riding coordinates:
 C02U(H02U), C02X(H02X), C030(H030), C032(H032), C033(H033), C034(H034),
 C035(H035), C038(H038), C03A(H03E), C03D(H03H), C03F(H03I), C03H(H03J),
 C03J(H03K), C03L(H03L), C03M(H03M), C03N(H03N)
7.c X=CH2 refined with riding coordinates:
 N02N(H02A,H02B), N02O(H02C,H02D), N02R(H02E,H02F), N02T(H02G,H02H), N02W(H02I,
 H02J), N031(H03A,H03B), N037(H03C,H03D), N03C(H03F,H03G)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83070
_shelx_fab_checksum              32832
_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 2.140
_oxdiff_exptl_absorpt_empirical_full_min 0.701