Dichlorooxo(<i>N,N</i>',<i>N</i>''-trimethyl-1,4,7-triazacyclononane-κ^3^<i>N</i>)vanadium(IV)
Dorothea Fiedler; Ognjen S. Miljanić; Eric J. Welch; Acta Crystallographica Section E 58 (2002) m347–m348; doi:10.1107/S160053680201053X

data_2201539
_publ_section_title
Dichlorooxo(<i>N,N</i>',<i>N</i>''-trimethyl-1,4,7-triazacyclononane-\k^3^<i>N</i>)vanadium(IV)
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m347
_journal_page_last               m348
_journal_paper_doi               10.1107/S160053680201053X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[V Cl2 O (C9 H21 N3)]'
_chemical_formula_moiety         'C9 H21 Cl2 N3 O V'
_chemical_formula_sum            'C9 H21 Cl2 N3 O V'
_chemical_formula_weight         309.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.000(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6069(15)
_cell_length_b                   7.7759(8)
_cell_length_c                   12.6586(14)
_cell_measurement_reflns_used    5166
_cell_measurement_temperature    141(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.73
_cell_volume                     1339.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1995)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.87
_diffrn_measurement_device       'Siemens SMART  CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5156
_diffrn_reflns_theta_full        24.7
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.760
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.760
_refine_ls_restrained_S_obs      0.718
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.XXXXP)^2^+0.XXXXP] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1219
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                1929
_reflns_number_total             2167
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6133.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201539