Tri-, tetra- and octa-metallic vanadium(III) clusters from new, simple starting materials: interplay of exchange and anisotropy effects
Tidmarsh, Ian S.; Batchelor, Luke J.; Scales, Emma; Laye, Rebecca H.; Sorace, Lorenzo; Caneschi, Andrea; Schnack, Jürgen; McInnes, Eric J. L.; Dalton Transactions  (2009) 9402–9409; doi:10.1039/b911586b

data_7002681
_publ_section_title
;
 Tri-, tetra- and octa-metallic vanadium(III) clusters from new, simple
 starting materials: interplay of exchange and anisotropy effects
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              9402
_journal_page_last               9409
_journal_paper_doi               10.1039/b911586b
_journal_year                    2009
_chemical_formula_moiety         '[V4Cl6(tmp)2(bipy)3]2.5MeCN'
_chemical_formula_sum            'C47 H53.5 Cl6 N8.5 O6 V4'
_chemical_formula_weight         1249.94
_chemical_name_common            sy
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.295(3)
_cell_angle_beta                 78.009(3)
_cell_angle_gamma                65.219(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8469(4)
_cell_length_b                   12.7487(5)
_cell_length_c                   19.7931(8)
_cell_measurement_reflns_used    8586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9250
_cell_measurement_theta_min      2.6935
_cell_volume                     2653.4(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Oxford Diffraction Xcaliber 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27231
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.6243
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         15797
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                10256
_reflns_number_total             15797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911586b.txt
_cod_data_source_block           oejlm244profp-1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2653.43(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C47 H53.50 Cl6 N8.50 O6 V4'
_cod_database_code               7002681