The twinned structure of the μ-isopropoxidodiisopropoxido(<i>p</i>-tolylimido)vanadium(V) dimer, twin refinement against CCD area-detector data
Lutz, Martin; Hagen, Henk; Schreurs, Antoine M.M.; Spek, Anthony L.; van Koten, Gerard; Acta Crystallographica Section C 55 (1999) 1636–1639; doi:10.1107/S0108270199003728

data_2009009
_publ_section_title
;
 The twinned structure of the
 \m-isopropoxidodiisopropoxido(<i>p</i>-tolylimido)vanadium(V) dimer,
 twin refinement against CCD area-detector data
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1636
_journal_page_last               1639
_journal_paper_doi               10.1107/S0108270199003728
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[V2 (C7 H7 N)2 (C3 H7 O)6]'
_chemical_formula_moiety         'C32 H56 N2 O6 V2'
_chemical_formula_sum            'C32 H56 N2 O6 V2'
_chemical_formula_weight         666.67
_chemical_melting_point          316
_chemical_name_systematic
;
bis((\m^2^-Isopropoxo)-di-isopropoxy-4-Methylphenylimido-vanadium(v))
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.297(4)
_cell_angle_beta                 71.869(4)
_cell_angle_gamma                61.3013(18)
_cell_formula_units_Z            1
_cell_length_a                   9.7491(6)
_cell_length_b                   10.0291(6)
_cell_length_c                   11.1681(5)
_cell_measurement_temperature    150(2)
_cell_volume                     907.28(9)
_computing_cell_refinement       'see above'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'see above'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.015
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18748
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         18748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.070
_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^)+(0.0378P)^2^+3.2555P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.174
_reflns_number_gt                16570
_reflns_number_total             18748
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1541.cif
_cod_data_source_block           s2004a
_cod_database_code               2009009
_cod_database_fobs_code          2009009