Site-selectivity in the halogenation of titanium-functionalized polyoxovanadate-alkoxide clusters.
VanGelder, L. E.; Forrestel, P. L.; Brennessel, W. W.; Matson, E. M.; Chemical communications (Cambridge, England) 54 (2018) 6839–6842; doi:10.1039/c8cc01517a

data_7121540
_publ_section_title
;
 Site-selectivity in the halogenation of titanium-functionalized
 polyoxovanadate-alkoxide clusters.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6839
_journal_page_last               6842
_journal_paper_doi               10.1039/c8cc01517a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C14 H42 Cl O18 Ti2 V4, Al Cl4, 1.5(C4 H8 O)'
_chemical_formula_sum            'C20 H54 Al Cl5 O19.5 Ti2 V4'
_chemical_formula_weight         1110.42
_chemical_name_common            matlv10
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-02-22 deposited with the CCDC.
2018-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3992(19)
_cell_length_b                   11.6179(11)
_cell_length_c                   19.5185(19)
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.24
_cell_volume                     4368.7(7)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            110728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.508
_diffrn_reflns_theta_max         30.542
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.971
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         13948
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+8.8422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8655
_reflns_number_total             13948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01517a2.cif
_cod_data_source_block           matlv10
_cod_depositor_comments
'Adding full bibliography for 7121539--7121540.cif.'
_cod_original_formula_sum        'C20 H54 Al Cl5 O19.50 Ti2 V4'
_cod_database_code               7121540
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.574
_shelx_estimated_absorpt_t_max   0.800
_shelx_res_checksum              7322