Peroxido Complexes of Vanadium(V) as Ligands. Crystal Structures of [Cd(NH3)6][{VO(O2)2(OH)}2{μ-Cd(NH3)4}] and [{VO(O2)2(Im)}2{μ-Cu(Im)4}] (Im = Imidazole).
Bystrický, Roman; Antal, Peter; Tatiersky, Jozef; Schwendt, Peter; Gyepes, Róbert; Zák, Zdirad; Inorganic chemistry 53 (2014) 5037–5043; doi:10.1021/ic500066p

data_4338318
_publ_section_title
;
 Peroxido Complexes of Vanadium(V) as Ligands. Crystal Structures of
 [Cd(NH3)6][{VO(O2)2(OH)}2{\m-Cd(NH3)4}] and [{VO(O2)2(Im)}2{\m-Cu(Im)4}]
 (Im = Imidazole).
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5037
_journal_page_last               5043
_journal_paper_doi               10.1021/ic500066p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '[Cd(NH3)6][{VO(O2)2(NH3)}2{mu-Cd(NH3)4}]'
_chemical_formula_sum            'Cd2 H32 N10 O12 V2'
_chemical_formula_weight         691.04
_chemical_name_systematic
; 
hexaammminecadmium(2+) 
bis[ammineoxidodiperoxidovadatato(V)]tetraamminecadmiumate(2-)
;
_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                82.906(3)
_cell_angle_beta                 87.456(2)
_cell_angle_gamma                61.540(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4932(2)
_cell_length_b                   7.5385(2)
_cell_length_c                   10.6984(3)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1574
_cell_measurement_theta_min      3.0851
_cell_volume                     527.15(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
;
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       omega-scan
_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  0.0068
_diffrn_reflns_av_sigmaI/netI    0.0062
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6054
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'after every 100 frames'
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  0.6689
_exptl_absorpt_correction_T_min  0.3885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0227P)^2^+1.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                1764
_reflns_number_total             1832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500066p_si_002.cif
_cod_data_source_block           cdvn
_cod_depositor_comments
'Adding full bibliography for 4338317--4338318.cif.'
_cod_original_cell_volume        527.15(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H32 Cd2 N10 O12 V2'
_cod_database_code               4338318