An 18-connected wheel-shaped molybdenum(V) nickel-phosphate cluster for photoelectrochemical sensing of levofloxacin.
Wang, Jie-Fei; Yin, Chun-Xiao; Qi, Jia-Xin; Ma, Yuan-Yuan; Lin, Zheng-Guo; Han, Zhan-Gang; Chemical communications (Cambridge, England) 61 (2025) 1914–1917; doi:10.1039/d4cc06389a

data_7134069
_publ_section_title
;
 An 18-connected wheel-shaped molybdenum(V) nickel-phosphate cluster for
 photoelectrochemical sensing of levofloxacin.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1914
_journal_page_last               1917
_journal_paper_doi               10.1039/d4cc06389a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C72.25 H72.5 Mo8 N24 Ni8.5 O67 P12, H6 Ni0.5 O3'
_chemical_formula_sum            'C72.25 H78.5 Mo8 N24 Ni9 O70 P12'
_chemical_formula_weight         4070.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-11-19 deposited with the CCDC.	2024-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                112.614(4)
_cell_angle_beta                 102.679(4)
_cell_angle_gamma                104.922(4)
_cell_formula_units_Z            2
_cell_length_a                   19.5356(11)
_cell_length_b                   20.8084(9)
_cell_length_c                   21.3316(7)
_cell_measurement_reflns_used    13589
_cell_measurement_temperature    297.0(4)
_cell_measurement_theta_max      75.6050
_cell_measurement_theta_min      2.3570
_cell_volume                     7224.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.0(4)
_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 0.998
_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   -120.00 -58.00   0.50    4.00    --  -49.01 -32.00 149.00  124
  2  \w    -31.00  12.00   0.50    4.00    --  -49.01  32.00 -51.00   86
  3  \w     41.00 120.00   0.50    4.00    --   49.01  32.00 -51.00  158
  4  \w    -23.00  10.00   0.50    4.00    --   49.01 -32.00 149.00   66
  5  \w   -138.00 -96.00   0.50    7.00    --  -90.00 -32.00 149.00   84
  6  \w    102.00 169.00   0.50    7.00    --  108.67  32.00 -51.00  134
  7  \w    -22.00  21.00   0.50    4.00    --  -49.01  19.00  90.00   86
  8  \w    -82.00 -13.00   0.50    4.00    --  -49.01 125.00-150.00  138
  9  \w    -22.00   8.00   0.50    4.00    --  -49.01  19.00  60.00   60
 10  \w   -100.00 -74.00   0.50    4.00    --  -49.01-125.00-120.00   52
 11  \w    -12.00  43.00   0.50    4.00    --   49.01 -38.00  30.00  110
 12  \w     49.00  89.00   0.50    4.00    --   49.01-125.00-150.00   80
 13  \w   -163.00-127.00   0.50    7.00    --  -90.00 -19.00 -60.00   72
 14  \w   -123.00 -79.00   0.50    7.00    --  -90.00 -19.00  90.00   88
 15  \w   -163.00-127.00   0.50    7.00    --  -90.00 -19.00  90.00   72
 16  \w   -160.00 -85.00   0.50    7.00    --  -90.00 -19.00   0.00  150
 17  \w    -85.00 -33.00   0.50    7.00    --  -90.00 125.00 150.00  104
 18  \w   -161.00-129.00   0.50    7.00    --  -90.00 -38.00  30.00   64
 19  \w    -83.00 -36.00   0.50    7.00    --  -90.00 125.00   0.00   94
 20  \w   -162.00 -83.00   0.50    7.00    --  -90.00 -38.00-120.00  158
 21  \w   -119.00 -89.00   0.50    7.00    --  -90.00 -99.00 -90.00   60
 22  \w   -108.00 -83.00   0.50    7.00    --  -90.00 -38.00  30.00   50
 23  \w    -47.00 -21.00   0.50    7.00    --  -90.00  57.00 120.00   52
 24  \w    -84.00 -58.00   0.50    7.00    --  -90.00  77.00 -30.00   52
 25  \w   -104.00 -79.00   0.50    7.00    --  -90.00 -19.00 -60.00   50
 26  \w     41.00  90.00   0.50    7.00    --  108.67 -99.00 150.00   98
 27  \w     57.00 111.00   0.50    7.00    --  108.67-125.00   0.00  108
 28  \w     40.00  96.00   0.50    7.00    --  108.67 -99.00  30.00  112
 29  \w     98.00 142.00   0.50    7.00    --  108.67  19.00-120.00   88
 30  \w     43.00  74.00   0.50    7.00    --  108.67-125.00  30.00   62
 31  \w    145.00 178.00   0.50    7.00    --  108.67  19.00-120.00   66
 32  \w     39.00  66.00   0.50    7.00    --  108.67 -57.00 -30.00   54
 33  \w     37.00  64.00   0.50    7.00    --  108.67 -57.00 -60.00   54
 34  \w     37.00  66.00   0.50    7.00    --  108.67 -57.00 -90.00   58
 35  \w     40.00  66.00   0.50    7.00    --  108.67 -57.00 150.00   52
 36  \w     54.00 100.00   0.50    7.00    --  108.67-125.00  90.00   92
 37  \w     81.00 111.00   0.50    7.00    --  108.67-125.00-180.00   60
 38  \w     51.00 124.00   0.50    7.00    --  108.67-142.00 139.73  146
 39  \w     40.00  66.00   0.50    7.00    --  108.67 -57.00-120.00   52
 40  \w     41.00  84.00   0.50    7.00    --  108.67 -99.00 120.00   86
 41  \w     74.00 108.00   0.50    7.00    --  108.67-115.00  27.32   68
 42  \w     81.00 106.00   0.50    7.00    --  108.67 -99.00 -90.00   50
 43  \w     40.00  66.00   0.50    7.00    --  108.67 -99.00 -90.00   52
 44  \w     63.00 105.00   0.50    7.00    --  108.67 -99.00-120.00   84
 45  \w     54.00 108.00   0.50    7.00    --  108.67-112.00 -42.17  108
 46  \w     49.00 108.00   0.50    7.00    --  108.67-109.00-172.94  118
 47  \w     40.00  66.00   0.50    7.00    --  108.67 -57.00-180.00   52
 48  \w     37.00  66.00   0.50    7.00    --  108.67 -57.00  30.00   58
 49  \w     54.00 108.00   0.50    7.00    --  108.67-115.00-106.35  108
;
_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      -0.0359546000
_diffrn_orient_matrix_UB_12      -0.0493271000
_diffrn_orient_matrix_UB_13      0.0316655000
_diffrn_orient_matrix_UB_21      0.0712564000
_diffrn_orient_matrix_UB_22      -0.0188350000
_diffrn_orient_matrix_UB_23      0.0146659000
_diffrn_orient_matrix_UB_31      0.0355459000
_diffrn_orient_matrix_UB_32      0.0687573000
_diffrn_orient_matrix_UB_33      0.0761402000
_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  0.1342
_diffrn_reflns_av_unetI/netI     0.1151
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.134
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1722
_refine_ls_number_reflns         24525
_refine_ls_number_restraints     7222
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.1120
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3062
_refine_ls_wR_factor_ref         0.3466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13881
_reflns_number_total             24525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06389a2.cif
_cod_data_source_block           111
_cod_depositor_comments          'Adding full bibliography for 7134069.cif.'
_cod_original_cell_volume        7224.9(6)
_cod_original_formula_sum        'C72.25 H78.50 Mo8 N24 Ni9 O70 P12'
_cod_database_code               7134069
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     'Ni C N O P Mo '
_shelx_estimated_absorpt_t_max   0.372
_shelx_estimated_absorpt_t_min   0.272
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N15-C91
 1.55 with sigma of 0.01
 C91-C79
 1.55 with sigma of 0.01
 N11-C75
 1.55 with sigma of 0.01
 C75-C38
 1.55 with sigma of 0.01
 C79-N15
 2.532 with sigma of 0.04
 Ni1-H35A \\sim Ni1-H35B
 with sigma of 0.02
 Ni1-H69A \\sim Ni1-H69B
 with sigma of 0.02
 Ni1-H67A \\sim Ni1-H67B
 with sigma of 0.02
3. Rigid bond restraints
 N3, N19, N6, N13, C1, C2, N4, C6, C15, C29, C31, C59, C61, C62, C63, C64, C65,
  C66, C68, C70, C72, C74, C76, N78
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N2, N23, C11, N17, C21, C33, C41, C43, C67, C83, C85, C87
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O18
\\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26
\\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34
\\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43
\\sim O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim O50 \\sim O51
\\sim O52 \\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim O57 \\sim O58 \\sim O59
\\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim O65 \\sim O66 \\sim O68
\\sim O70 \\sim O72 \\sim O17 \\sim O35 \\sim O67 \\sim O69 \\sim O71: within
5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 5A
C49 \\sim C46 \\sim C33 \\sim C67 \\sim C74 \\sim C76 \\sim C1 \\sim C6 \\sim
C26 \\sim C30 \\sim C80 \\sim C84 \\sim C8 \\sim C12 \\sim C14 \\sim C18 \\sim
C22 \\sim C24 \\sim C7 \\sim C19 \\sim C77 \\sim C39 \\sim C79 \\sim C5 \\sim
C81 \\sim C25 \\sim C51 \\sim C13 \\sim C53 \\sim C27 \\sim C55 \\sim C29 \\sim
C32 \\sim C34 \\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C41 \\sim C48 \\sim
C50 \\sim C52 \\sim C54 \\sim C56 \\sim C58 \\sim C57 \\sim C59 \\sim C15 \\sim
C61 \\sim C31 \\sim C63 \\sim C2 \\sim C60 \\sim C62 \\sim C64 \\sim C66 \\sim
C68 \\sim C70 \\sim C72 \\sim C65 \\sim C69 \\sim C35 \\sim C71 \\sim C9 \\sim
C73 \\sim C37 \\sim C75 \\sim C83 \\sim C21 \\sim C85 \\sim C43 \\sim C87 \\sim
C11 \\sim C86 \\sim C88 \\sim C90 \\sim C45 \\sim C23 \\sim C47 \\sim C3 \\sim
C91 \\sim N1 \\sim N44 \\sim N18 \\sim N2 \\sim N23 \\sim N17 \\sim N3 \\sim
N13 \\sim N78 \\sim N19 \\sim N4 \\sim N6 \\sim N5 \\sim N28 \\sim N11 \\sim N7
\\sim N15 \\sim N82 \\sim N8 \\sim N10 \\sim N22 \\sim N12 \\sim N14 \\sim N16
\\sim N21 \\sim N20 \\sim N9: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 5A
5. Others
 Fixed Sof: P3(0.5) P5(0.5) P11(0.5) P13(0.5) N1(0.75) C49(0.75) H49(0.75)
 N44(0.75) H44(0.75) N18(0.75) C46(0.75) H46(0.75) N2(0.5) C33(0.5) H33(0.5)
 N23(0.5) C67(0.5) H67(0.5) N17(0.5) H17(0.5) N7(0.75) C80(0.75) H80(0.75)
 N15(0.75) N82(0.75) H82(0.75) C84(0.75) H84(0.75) C7(0.75) H7A(0.75) H7B(0.75)
 C19(0.75) C77(0.75) H77(0.75) C39(0.75) H39(0.75) C79(0.75) C5(0.75) H5(0.75)
 C81(0.75) H81(0.75) C41(0.5) H41A(0.5) H41B(0.5) C69(0.75) C35(0.75) H35(0.75)
 C71(0.75) H71(0.75) C9(0.75) C73(0.75) H73(0.75) C37(0.75) H37(0.75) C83(0.5)
 C21(0.5) H21(0.5) C85(0.5) H85(0.5) C43(0.5) C87(0.5) H87(0.5) C11(0.5)
 H11(0.5) O17(0.5) H17A(0.5) H17B(0.5) O67(0.5) H67A(0.5) H67B(0.5) O69(0.5)
 H69A(0.5) H69B(0.5) O71(0.5) H71A(0.5) H71B(0.5)
6.a Riding coordinates:
 O35(H35A,H35B)
6.b Free rotating group:
 O67(H67A,H67B), O69(H69A,H69B)
6.c Rotating group:
 O17(H17A,H17B), O71(H71A,H71B)
6.d Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C29(H29A,H29B), C41(H41A,H41B), C57(H57A,H57B), C60(H60A,H60B),
 C65(H65A,H65B), C75(H75A,H75B), C86(H86A,H86B), C91(H91A,H91B)
6.e Aromatic/amide H refined with riding coordinates:
 C49(H49), N44(H44), C46(H46), C33(H33), C67(H67), N17(H17), C74(H74),
 C76(H76), N78(H78), C1(H1), N4(H4), C6(H6), C26(H26), N28(H28), C30(H30),
 C80(H80), N82(H82), C84(H84), C8(H8), N10(H10), C12(H12), C14(H14), N16(H16),
 C18(H18), N20(H20), C22(H22), C24(H24), C77(H77), C39(H39), C5(H5), C81(H81),
 C51(H51), C13(H13), C27(H27), C55(H55), C34(H34), C36(H36), C40(H40), C42(H42),
  C50(H50), C52(H52), C56(H56), C58(H58), C59(H59), C15(H15), C31(H31),
 C63(H63), C64(H64), C66(H66), C70(H70), C72(H72), C35(H35), C71(H71), C73(H73),
  C37(H37), C21(H21), C85(H85), C87(H87), C11(H11), C90(H90), C45(H45),
 C47(H47), C3(H3)
6.f Fitted pentagon refined as free rotating group:
 N1(C49,N44,N18,C46), N2(C33,N23,C67,N17), N3(C74,N13,C76,N78), N19(C1,N4,N6,
 C6), N5(C26,N28,N11,C30), N7(C80,N15,N82,C84), N8(C8,N10,N22,C12), N12(C14,N14,
 N16,C18), N21(N20,C22,N9,C24)
6.g Fitted hexagon refined as free rotating group:
 C19(C77,C39,C79,C5,C81), C25(C51,C13,C53,C27,C55), C32(C34,C36,C38,C40,C42),
 C48(C50,C52,C54,C56,C58), C59(C15,C61,C31,C63,C2), C62(C64,C66,C68,C70,C72),
 C69(C35,C71,C9,C73,C37), C83(C21,C85,C43,C87,C11), C88(C90,C45,C23,C47,C3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53967
_shelx_hkl_checksum              61854
_shelx_fab_checksum              24736
_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 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.496