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_7246891
_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 H34 Mn3 Mo12 N8 O66 P8'
_chemical_formula_weight         3054.45
_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                102.6370(10)
_cell_angle_beta                 106.00
_cell_angle_gamma                110.82
_cell_formula_units_Z            1
_cell_length_a                   11.9440(3)
_cell_length_b                   13.7940(4)
_cell_length_c                   14.6825(4)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     2033.94(10)
_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      296.15
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0142
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15066
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         1.542
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.504
_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    2.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.057
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10093
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0561P)^2^+13.2540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9100
_reflns_number_total             10093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00517h2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7246890--7246891.cif.'
_cod_database_code               7246891
_shelx_shelxl_version_number     2018/3
_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
 C9-C7
 1.5 with sigma of 0.01
 C18-C13
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O32) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 N4, N3, C7, C9, C8, C10, C12, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, N5, C18, C13, C14, C17, C15, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O32(0.5) O33(0.5) O34(0.5) O35(0.5) N3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8(0.5) C9(0.5) C10(0.5) H10(0.5)
 C11(0.5) H11(0.5) N4(0.5) H4(0.5) C12(0.5) H12(0.5) N5(0.5) H7C(0.5) H5A(0.5)
 H5B(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) N6(0.5) H6(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18A(0.5) H18B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C18(H18A,H18B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4A), C5(H5), C6(H6A), C8(H8), C10(H10), C11(H11), N4(H4),
 C12(H12), C14(H14), C15(H15), N6(H6), C16(H16), C17(H17)
6.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,N4,C12), C13(C14,C15,N6,C16,C17)
6.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C), N5(H7C,H5A,H5B)
;
_shelx_res_checksum              34603
_shelx_hkl_checksum              95439
_olex2_submission_special_instructions 'No special instructions were received'