Halide encapsulation by dicarboxylate oxido-vanadium cage complexes.
Gómez, Margarita; Pastor, Antonio; Álvarez, Eleuterio; Olloqui-Sariego, José Luis; Galindo, Agustín; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2183–2191; doi:10.1039/c7dt04251e

data_7045248
_publ_section_title
;
 Halide encapsulation by dicarboxylate oxido-vanadium cage complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2183
_journal_page_last               2191
_journal_paper_doi               10.1039/c7dt04251e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C16 H16 O36 V8, 2(C16 H36 N), 3(C2 H3 N), 2(Cl)'
_chemical_formula_sum            'C54 H97 Cl2 N5 O36 V8'
_chemical_formula_weight         1870.78
_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-2016/6
_audit_update_record
;
2017-09-07 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.9530(10)
_cell_angle_beta                 117.9780(10)
_cell_angle_gamma                93.3520(10)
_cell_formula_units_Z            2
_cell_length_a                   16.3158(6)
_cell_length_b                   16.3786(6)
_cell_length_c                   16.7821(6)
_cell_measurement_reflns_used    8178
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.43
_cell_volume                     3948.8(3)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71065
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.957
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_correction_T_min  0.6767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.541
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         14200
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+5.2245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11860
_reflns_number_total             14200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04251e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045248--7045250.cif.'
_cod_database_code               7045248
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.677
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              76656