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_7123334
_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            'H62 Mo18 N4 O81 P2'
_chemical_formula_weight         3203.39
_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                82.099(3)
_cell_angle_beta                 87.537(3)
_cell_angle_gamma                83.277(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7650(8)
_cell_length_b                   15.5376(9)
_cell_length_c                   17.7625(10)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.32
_cell_volume                     3735.6(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 0.998
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.490
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    3.082
_exptl_absorpt_correction_T_max  0.4670
_exptl_absorpt_correction_T_min  0.3284
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    2.848
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.11
_refine_diff_density_rms         0.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         14635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0316P)^2^+31.9681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12133
_reflns_number_total             14635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02361e2.cif
_cod_data_source_block           nk1_70_nh4
_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               7123334
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.861
_shelx_res_checksum              15653
_shelx_hkl_checksum              91783