Facile and green synthesis of decatungstate-based nickel(ii) complex coated onto modified Fe3O4 nanoparticles with enhanced antimicrobial activity against antibiotic-resistant bacteria
Xing, Cuili; Ma, Pengtao; Zhao, Meng; Chang, Jiangnan; Guo, Xiaoyuan; Sun, Lin; Li, Mingxue; CrystEngComm 23 (2021) 3919–3928; doi:10.1039/D1CE00421B

data_7242744
_publ_section_title
;
 Facile and green synthesis of decatungstate-based nickel(ii) complex
 coated onto modified Fe3O4 nanoparticles with enhanced antimicrobial
 activity against antibiotic-resistant bacteria
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3919
_journal_page_last               3928
_journal_paper_doi               10.1039/D1CE00421B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'O32 W10, 4(O), 2(C16 H20 N8 Ni S2)'
_chemical_formula_sum            'C32 H40 N16 Ni2 O36 P0 S4 W10'
_chemical_formula_weight         3308.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-07 deposited with the CCDC.	2021-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.101(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3341(11)
_cell_length_b                   21.413(2)
_cell_length_c                   14.0095(13)
_cell_measurement_reflns_used    7439
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.24
_cell_volume                     3231.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         1.890
_exptl_absorpt_coefficient_mu    18.512
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1720 before and 0.0654 after correction. The Ratio of minimum to maximum transmission is 0.2673. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.985
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5750
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0494P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4827
_reflns_number_total             5750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00421b2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7242744.cif.'
_cod_original_cell_volume        3231.9(5)
_cod_database_code               7242744
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.357
_shelx_estimated_absorpt_t_min   0.045
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim W1 \\sim W5: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O11 \\sim W3 \\sim W4: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O15 \\sim W5: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O1) \\sim Ueq, Uanis(W1) \\sim Ueq, Uanis(W5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(W3) \\sim Ueq, Uanis(W4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(W5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C11(H11A,H11B,H11C)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), C5(H5), C6(H6A), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
  C16(H16)
3.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N5(H5A,H5B)
;
_shelx_res_checksum              85323
_shelx_hkl_checksum              61652
_olex2_submission_special_instructions 'No special instructions were received'