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_7044314
_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         'C24 H36 N6 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H108 N8 O25 V6'
_chemical_formula_weight         1599.14
_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_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                73.992(2)
_cell_angle_beta                 71.464(2)
_cell_angle_gamma                78.819(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4733(17)
_cell_length_b                   11.9543(17)
_cell_length_c                   14.603(2)
_cell_measurement_reflns_used    1848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      2.44
_cell_volume                     1812.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.342
_diffrn_reflns_theta_min         1.511
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1235 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.8869. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.6840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5373
_reflns_number_total             7395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03376a2.cif
_cod_data_source_block           2f
_cod_original_cell_volume        1812.9(5)
_cod_database_code               7044314
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              82147