Di-μ-oxido-bis({2-[(<i>R</i>,<i>R</i>)-({-})-(2-aminocyclohexyl)iminomethyl]-4-nitrophenolato-κ^3^<i>N</i>,<i>N</i>',<i>O</i>}oxidovanadium(V)) dimethyl sulfoxide disolvate
Romanowski, Grzegorz; Wera, Michał; Sikorski, Artur; Acta Crystallographica Section E 65 (2009) m25–m26; doi:10.1107/S1600536808038762

data_2220545
_publ_section_title
;Di-\m-oxido-bis({2-[(<i>R</i>,<i>R</i>)-({-})-(2-aminocyclohexyl)iminomethyl]-4-nitrophenolato-\k^3^<i>N</i>,<i>N</i>',<i>O</i>}oxidovanadium(V))
 dimethyl sulfoxide disolvate
;
_journal_coeditor_code           HY2164
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m25
_journal_page_last               m26
_journal_paper_doi               10.1107/S1600536808038762
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[V2 (C13 H16 N3 O3)2 O4], 2C2 H6 O S'
_chemical_formula_moiety         'C26 H32 N6 O10 V2, 2(C2 H6 O S)'
_chemical_formula_sum            'C30 H44 N6 O12 S2 V2'
_chemical_formula_weight         846.71
_chemical_name_systematic
;
Di-\m-oxido-bis({2-[(<i>R</i>,<i>R</i>)-(-)-(2-aminocyclohexyl)iminomethyl]-
4-nitrophenolato-\k^3^<i>N</i>,<i>N</i>',<i>O</i>}oxidovanadium(V))
dimethyl sulfoxide disolvate
;
_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                77.69(3)
_cell_angle_beta                 88.62(3)
_cell_angle_gamma                76.13(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2490(10)
_cell_length_b                   11.747(2)
_cell_length_c                   11.809(2)
_cell_measurement_reflns_used    3355
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.03
_cell_volume                     953.4(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.4002
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction Ruby CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6786
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.71964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.442
_refine_ls_extinction_coef       0.0061(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.444
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+4.2049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                3245
_reflns_number_total             3355
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2164.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2220545
_cod_database_fobs_code          2220545