The Cu(I)-catalysed Huisgen 1,3-dipolar cycloaddition route to (bio-)organic functionalisation of polyoxovanadates
Linnenberg, Oliver; Kondinski, Aleksandar; Stöcker, Cornelia; Monakhov, Kirill; Dalton Trans.  (2017) –; doi:10.1039/C7DT03376A

data_7044313
_publ_section_title
;
 The Cu(I)-catalysed Huisgen 1,3-dipolar cycloaddition route to
 (bio-)organic functionalisation of polyoxovanadates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03376A
_journal_year                    2017
_chemical_formula_moiety         'C16 H22 O21 V6 2(C16 H36 N)'
_chemical_formula_sum            'C48 H94 N2 O21 V6'
_chemical_formula_weight         1340.89
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.834(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.244(2)
_cell_length_b                   22.208(3)
_cell_length_c                   15.317(2)
_cell_measurement_reflns_used    1445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.53
_cell_measurement_theta_min      2.37
_cell_volume                     5844.9(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29328
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.163
_diffrn_reflns_theta_max         24.163
_diffrn_reflns_theta_min         1.185
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1703 before and 0.0780 after correction.
The Ratio of minimum to maximum transmission is 0.8162.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         9334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0510
_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^)+0.0396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6652
_reflns_number_total             9334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03376a2.cif
_cod_data_source_block           1
_cod_database_code               7044313
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              57507