Two new manganese-based phosphomolybdate compounds as electrochemical sensors for the highly sensitive trace determination of heavy metal Cr(vi) ions
Wang, Jinling; Liu, Xiaohui; Chang, Zhihan; Xu, Na; Wang, Xiuli; CrystEngComm 25 (2023) 3953–3958; doi:10.1039/D3CE00517H

data_7246890
_publ_section_title
;
 Two new manganese-based phosphomolybdate compounds as electrochemical
 sensors for the highly sensitive trace determination of heavy metal
 Cr(vi) ions
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              3953
_journal_page_last               3958
_journal_paper_doi               10.1039/D3CE00517H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Mn3 Mo12 O66 P8, 4(C6 H10 N2)'
_chemical_formula_sum            'C24 H40 Mn3 Mo12 N8 O66 P8'
_chemical_formula_weight         3060.50
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-11-01 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.2760(10)
_cell_angle_beta                 106.7290(10)
_cell_angle_gamma                110.0090(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0309(8)
_cell_length_b                   13.9974(9)
_cell_length_c                   14.7291(9)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     2078.4(2)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15078
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         1.813
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.451
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1467
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.753
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         10204
_refine_ls_number_restraints     957
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0553P)^2^+17.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9434
_reflns_number_total             10204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00517h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7246890--7246891.cif.'
_cod_database_code               7246890
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.591
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2. Restrained distances
 C17-C18
 1.4 with sigma of 0.01
 N2-C18
 1.5 with sigma of 0.01
 N6-C24 = N5-C7
 1.4 with sigma of 0.01
 C19-C24
 1.5 with sigma of 0.01
3. Restrained planarity
 N4, C13, C14, C15, C16, C17, C18
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C13 \\sim C14 \\sim C15
\\sim C16 \\sim C17 \\sim C18 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11
\\sim C12 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8: within 3.2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.2A
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N1, N2, N3, N4, C1, C2, C3, C4, C5, C6, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: O32(0.75) O33(0.65) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N2(0.5)
 H2A(0.5) H2B(0.5) H2C(0.5) C1(0.5) H1(0.5) C2(0.5) C3(0.5) H3(0.5) N3(0.5)
 H3A(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6A(0.5) H6B(0.5) C13(0.5)
 H13(0.5) N4(0.5) H4A(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) N5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) N6(0.5) H6C(0.5) H6D(0.5) H6E(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5)
 H8(0.5) C9(0.5) H9(0.5) C10(0.5) C11(0.5) H11(0.5) N7(0.5) H7(0.5) C12(0.5)
 H12(0.5) C19(0.5) C20(0.5) H20(0.5) N8(0.5) H8A(0.5) C21(0.5) H21(0.5)
 C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5) H24B(0.5) O35(0.25)
 O34(0.35)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C7(H7A,H7B), C24(H24A,H24B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), N3(H3A), C4(H4), C5(H5), C13(H13), N4(H4A), C14(H14),
 C15(H15), C16(H16), C8(H8), C9(H9), C11(H11), N7(H7), C12(H12), C20(H20),
 N8(H8A), C21(H21), C22(H22), C23(H23)
7.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,N3,C4,C5), C13(N4,C14,C15,C16,C17), C8(C9,C10,C11,N7,C12), C19(C20,
 N8,C21,C22,C23)
7.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N5(H5A,H5B,H5C), N6(H6C,H6D,H6E)
;
_shelx_res_checksum              80571
_shelx_hkl_checksum              31581
_olex2_submission_special_instructions 'No special instructions were received'