Dichlorobis(tetrahydrofuran)(<i>N,N</i>'-di-<i>tert</i>-butylethane-1,2-diamine)vanadium(II)
Niedwieski, Antonio Carlos; Leigh, G. Jeffery; Hasegawa, Tai; Nunes, Fábio Souza; Acta Crystallographica Section E 59 (2003) m939–m941; doi:10.1107/S1600536803019743

data_2202277
_publ_section_title
Dichlorobis(tetrahydrofuran)(<i>N,N</i>'-di-<i>tert</i>-butylethane-1,2-diamine)vanadium(II)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m939
_journal_page_last               m941
_journal_paper_doi               10.1107/S1600536803019743
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[V (C4 H8 O)2 (C8 H22 N2) Cl2]'
_chemical_formula_moiety         'C18 H38 Cl2 N2 O2 V'
_chemical_formula_sum            'C18 H38 Cl2 N2 O2 V'
_chemical_formula_weight         436.34
_chemical_name_common            '[VCl2(thf)2(tBuNCH2CH2NtBu)]'
_chemical_name_systematic
;
Dichlorobis(tetrahydrofuran)N,N'-di-tert-buthylethane-1,2-diaminevanadium(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.236(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.915(2)
_cell_length_b                   10.3733(9)
_cell_length_c                   11.4042(13)
_cell_measurement_reflns_used    16335
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_volume                     2273.5(4)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor,1997) and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia,1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8029
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, 1995
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0475P)^2^+4.9995P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                2003
_reflns_number_total             2597
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ac6058.cif
_cod_data_source_block           I
_cod_original_cell_volume        2273.6(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202277
_cod_database_fobs_code          2202277