M(C(6)H(16)N(3))(2)(VO(3))(4) as heterogeneous catalysts. Study of three new hybrid vanadates of cobalt(ii), nickel(ii) and copper(ii) with 1-(2-aminoethyl)piperazonium.
Larrea, Edurne S.; Mesa, José L; Pizarro, José L; Iglesias, Marta; Rojo, Teófilo; Arriortua, María I; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12690–12698; doi:10.1039/c1dt10971e

data_7017301
_publ_section_title
;
 M(C(6)H(16)N(3))(2)(VO(3))(4) as heterogeneous catalysts. Study of three
 new hybrid vanadates of cobalt(ii), nickel(ii) and copper(ii) with
 1-(2-aminoethyl)piperazonium.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12690
_journal_page_last               12698
_journal_paper_doi               10.1039/c1dt10971e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C6 H16 Co0.5 N3 O6 V2'
_chemical_formula_weight         357.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-02-10T11:40:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.542(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8810(10)
_cell_length_b                   9.4000(10)
_cell_length_c                   15.024(2)
_cell_measurement_reflns_used    15027
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      2.26
_cell_volume                     1248.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24283
_diffrn_reflns_theta_full        29.78
_diffrn_reflns_theta_max         29.78
_diffrn_reflns_theta_min         2.87
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.159
_exptl_absorpt_correction_T_max  0.8989
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-SHAPE'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_meas      1.90(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.024
_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^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0396
_reflns_number_gt                2696
_reflns_number_total             3531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10971e.txt
_cod_data_source_block           co_95
_cod_original_cell_volume        1248.4(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C6 H16 Co0.50 N3 O6 V2'
_cod_database_code               7017301