A simple one-step synthetic route to access a range of metal-doped polyoxovanadate clusters.
Lu, Haijiao; Jethwa, Rajesh B.; Jenkinson, Kellie J.; Wheatley, Andrew E. H.; Hao, Hongxun; Wright, Dominic S.; Pike, Sebastian D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4555–4564; doi:10.1039/c8dt05072d

data_7049248
_publ_section_title
;
 A simple one-step synthetic route to access a range of metal-doped
 polyoxovanadate clusters.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4555
_journal_page_last               4564
_journal_paper_doi               10.1039/c8dt05072d
_journal_volume                  48
_journal_year                    2019
_chemical_compound_source        '301, Dept Chem, Uni Cambridge'
_chemical_formula_moiety         'C15.00 H45 Bi1 Br0.50 Co0.25 O24 S7.50 V6'
_chemical_formula_sum            'C15 H45 Bi Br0.5 Co0.25 O24 S7.5 V6'
_chemical_formula_weight         1419.32
_chemical_name_systematic        '[Bi2(DMSO)6V12O33Br]2[Co(DMSO)6]11DMSO'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-11-24
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2018-12-20 deposited with the CCDC.    2019-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                119.4423(12)
_cell_angle_beta                 91.5191(13)
_cell_angle_gamma                107.3877(13)
_cell_formula_units_Z            4
_cell_length_a                   17.5652(5)
_cell_length_b                   17.6114(5)
_cell_length_c                   17.7741(5)
_cell_measurement_reflns_used    56332
_cell_measurement_temperature    180
_cell_measurement_theta_max      134
_cell_measurement_theta_min      5
_cell_volume                     4468.9(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52365
_diffrn_reflns_theta_full        67.018
_diffrn_reflns_theta_max         67.018
_diffrn_reflns_theta_min         2.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.824
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2769
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.47
_refine_diff_density_min         -4.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         14809
_refine_ls_number_restraints     822
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.0245707
_refine_ls_shift/su_mean         0.0009999
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1600
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1600
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              18
_reflns_limit_k_min              -21
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                12451
_reflns_number_total             15785
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.43
_oxford_diffrn_Wilson_scale      612.62
_oxford_refine_ls_r_factor_ref   0.0762
_oxford_refine_ls_scale          0.059719(11)
_oxford_reflns_number_all        14809
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B1_0058 in P-1'
_cod_data_source_file            c8dt05072d2.cif
_cod_data_source_block           2Br-Co
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049248--7049252.cif.
;
_cod_original_cell_volume        4468.89(13)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C15.00 H45 Bi1 Br0.50 Co0.25 O24 S7.50 V6'
_cod_database_code               7049248