Two new polyoxometalate-based metal-organic complexes for the detection of trace Cr(VI) and their capacitor performance.
Liu, Qian-Qian; Wang, Xiu-Li; Lin, Hong-Yan; Chang, Zhi-Han; Zhang, Yu-Chen; Tian, Yuan; Lu, Jun-Jun; Yu, Le; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9450–9456; doi:10.1039/d1dt01247a

data_7707694
_publ_section_title
;
 Two new polyoxometalate-based metal-organic complexes for the detection
 of trace Cr(VI) and their capacitor performance.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9450
_journal_page_last               9456
_journal_paper_doi               10.1039/d1dt01247a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Mo12 O40 P, C24 H32 Cu2 N12 O8, 2(H2 O)'
_chemical_formula_sum            'C24 H36 Cu2 Mo12 N12 O50 P'
_chemical_formula_weight         2601.98
_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             2020-10-22
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-11-11 deposited with the CCDC.	2021-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                67.854(2)
_cell_angle_beta                 74.137(2)
_cell_angle_gamma                75.682(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6974(14)
_cell_length_b                   11.8807(13)
_cell_length_c                   12.1832(14)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1488.6(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.734
_diffrn_reflns_theta_min         1.834
_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    3.287
_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    2.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1241
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.076
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0229P)^2^+9.4230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5049
_reflns_number_total             6966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01247a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707694--7707695.cif.'
_cod_database_code               7707694
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1Wa-H3Wa
 2.4 with sigma of 0.01
 Cu1-H1Wa \\sim Cu1-H1Wb
 with sigma of 0.02
3. Others
 Fixed Sof: O24(0.5) O25(0.5) O26(0.5) O27(0.5)
4.a Free rotating group:
 O1W(H1Wa,H1Wb), O3W(H3Wa,H3Wb)
4.b Rotating group:
 O2W(H2Wa,H2Wb)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C11(H11a,H11b)
4.d Aromatic/amide H refined with riding coordinates:
 N6(H6), N5(H5), C2(H2), C8(H8), C1(H1), C7(H7), C3(H3), C6(H6a)
;
_shelx_res_checksum              29279
_shelx_hkl_checksum              64280
_olex2_submission_special_instructions 'No special instructions were received'