Non-oxo vanadium(IV) alkoxide chemistry: solid state structures, aggregation equilibria and thermochromic behaviour in solution.
Westrup, Kátia C M; Gregório, Thaiane; Stinghen, Danilo; Reis, Dayane M.; Hitchcock, Peter B.; Ribeiro, Ronny R.; Barison, Andersson; Back, Davi F.; de Sá, Eduardo L; Nunes, Giovana G.; Soares, Jaísa F; Dalton transactions (Cambridge, England : 2003) 40 (2011) 3198–3210; doi:10.1039/c0dt01547d

data_7015368
_publ_section_title
;
 Non-oxo vanadium(IV) alkoxide chemistry: solid state structures,
 aggregation equilibria and thermochromic behaviour in solution.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3198
_journal_page_last               3210
_journal_paper_doi               10.1039/c0dt01547d
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H88 O8 V2'
_chemical_formula_sum            'C40 H88 O8 V2'
_chemical_formula_weight         798.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-04-27T15:21:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                63.298(4)
_cell_angle_beta                 88.580(4)
_cell_angle_gamma                88.169(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9481(8)
_cell_length_b                   10.9738(7)
_cell_length_c                   11.4416(6)
_cell_measurement_reflns_used    19493
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1227.31(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia,1997)'
_computing_publication_material  'WinGX publication routines (Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.277134E-1
_diffrn_orient_matrix_UB_12      -0.815708E-1
_diffrn_orient_matrix_UB_13      -0.8513E-2
_diffrn_orient_matrix_UB_21      0.656276E-1
_diffrn_orient_matrix_UB_22      0.142458E-1
_diffrn_orient_matrix_UB_23      -0.669667E-1
_diffrn_orient_matrix_UB_31      0.572508E-1
_diffrn_orient_matrix_UB_32      -0.596131E-1
_diffrn_orient_matrix_UB_33      0.708215E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13642
_diffrn_reflns_theta_full        23.05
_diffrn_reflns_theta_max         23.05
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.9640
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.112
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+9.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3306
_refine_ls_wR_factor_ref         0.3377
_reflns_number_gt                2828
_reflns_number_total             3360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01547d.txt
_cod_data_source_block           apr2006
_cod_database_code               7015368