Control of Bridging Ligands in [(V2O3)2(RXO3)4⊂F]−Cage Complexes: A Unique Way To Tune Their Chemical Properties
Rabeah, Jabor; Dimitrov, Anton; Surkus, Annette-Enrica; Jiao, Haijun; Baumann, Wolfgang; Stößer, Reinhard; Radnik, Jörg; Bentrup, Ursula; Brückner, Angelika; Organometallics 33 (2014) 4905–; doi:10.1021/om500153d

data_4083011
_publ_section_title
;
 Control of Bridging Ligands in [(V2O3)2(RXO3)4&#x2282;F]&#x2212;Cage
 Complexes: A Unique Way To Tune Their Chemical Properties
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4905
_journal_paper_doi               10.1021/om500153d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H20 As4 O18 V4, C24 H20 P, C2 H3 N, F'
_chemical_formula_sum            'C50 H43 As4 F N O18 P V4'
_chemical_formula_weight         1499.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P -2bc -2c'
_space_group_name_H-M_alt        'P c 21 b'
_symmetry_space_group_name_Hall  'P -2bc -2c'
_symmetry_space_group_name_H-M   'P c 21 b'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6958(19)
_cell_length_b                   18.567(2)
_cell_length_c                   19.811(4)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.05
_cell_volume                     5405.6(14)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            90472
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.225
_diffrn_reflns_theta_min         2.045
_exptl_absorpt_coefficient_mu    3.208
_exptl_absorpt_correction_T_max  .463
_exptl_absorpt_correction_T_min  .307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Spek, 2003'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 5143 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         14398
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0344
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                12302
_reflns_number_total             14398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500153d_si_002.cif
_cod_data_source_block           VAsF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5405.4(14)
_cod_database_code               4083011
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.513
_shelxl_version_number           2013-4
_shelx_res_checksum              73364
_shelx_hkl_checksum              36872