Synthesis of Polyoxometalate Clusters using Carbohydrates as Reducing Agents Leads to Isomer-Selection
Cronin, Lee; Janusson, Eric; Kler, Noel; Vila-Nadal, Laia; Long, Deliang; Chemical Communications  (2019) –; doi:10.1039/C9CC02361E

data_7123335
_publ_section_title
;
 Synthesis of Polyoxometalate Clusters using Carbohydrates as Reducing
 Agents Leads to Isomer-Selection
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02361E
_journal_year                    2019
_chemical_formula_sum            'H52 Mo18 N6 O76 P2'
_chemical_formula_weight         3141.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                101.443(4)
_cell_angle_beta                 98.500(4)
_cell_angle_gamma                114.254(4)
_cell_formula_units_Z            2
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_cell_length_b                   14.4286(10)
_cell_length_c                   19.8131(14)
_cell_measurement_reflns_used    8194
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.34
_cell_volume                     3141.5(4)
_computing_cell_refinement       Apex3
_computing_data_collection       Apex3
_computing_data_reduction        Apex3
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45024
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.713
_diffrn_reflns_theta_min         1.616
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    3.657
_exptl_absorpt_correction_T_max  0.0921
_exptl_absorpt_correction_T_min  0.0544
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.321
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.70
_refine_diff_density_min         -1.05
_refine_diff_density_rms         0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         11933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0330P)^2^+10.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9373
_reflns_number_total             11933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02361e2.cif
_cod_data_source_block           nk1_57_c2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7123335
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.642
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              78258
_shelx_hkl_checksum              82153