Synthesis, structural characterisation, and cytotoxicity studies of Bi, W, and Mo containing homo- and hetero-bimetallic polyoxometalates.
Senevirathna, Dimuthu C.; Werrett, Melissa V.; Kubeil, Manja; Stephan, Holger; Andrews, Philip C.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15962–15969; doi:10.1039/c9dt03288f

data_7701295
_publ_section_title
;
 Synthesis, structural characterisation, and cytotoxicity studies of Bi,
 W, and Mo containing homo- and hetero-bimetallic polyoxometalates.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15962
_journal_page_last               15969
_journal_paper_doi               10.1039/c9dt03288f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C16 H54 Bi O8 S8, 2(Mo4 O13), H2 O, N H4'
_chemical_formula_sum            'C16 H54 Bi Mo8 N O35 S8'
_chemical_formula_weight         2053.72
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-08 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.973(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6976(7)
_cell_length_b                   23.1883(13)
_cell_length_c                   20.2723(11)
_cell_measurement_reflns_used    65486
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.070
_cell_measurement_theta_min      2.419
_cell_volume                     5358.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65486
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.070
_diffrn_reflns_theta_min         2.419
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.481
_exptl_absorpt_correction_T_max  0.456
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12914
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0178P)^2^+5.6404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9796
_reflns_number_total             12914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03288f2.cif
_cod_data_source_block           DCPOM02
_cod_depositor_comments
'Adding full bibliography for 7701293--7701295.cif.'
_cod_database_code               7701295
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.456
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O35-H35B \\sim O35-H35A
 with sigma of 0.02
3. Others
 Sof(H8BD)=Sof(H8BE)=Sof(H8BF)=Sof(H7BD)=Sof(H7BE)=Sof(H7BF)=Sof(S4)=1-FVAR(1)
 Sof(S4')=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=FVAR(1)
4.a Free rotating group:
 O35(H35A)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C),
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C4(H4A,H4B,H4C), C8(H8AA,H8AB,H8AC),
 C8(H8BD,H8BE,H8BF), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C7(H7AA,H7AB,H7AC), C7(H7BD,H7BE,H7BF), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              1140
_olex2_submission_special_instructions 'No special instructions were received'