Construction of 3d−4f Mixed-Metal Complexes Based on a Binuclear Oxovanadium Unit: Synthesis, Crystal Structure, EPR, and Magnetic Properties
Shi, Wei; Chen, Xiao-Yan; Zhao, Bin; Yu, Ao; Song, Hai-Bin; Cheng, Peng; Wang, Hong-Gen; Liao, Dai-Zheng; Yan, Shi-Ping; Inorganic Chemistry 45 (2006) 3949–3957; doi:10.1021/ic051979y

data_4331983
_publ_section_title
;
 Construction of 3d&#x2212;4f Mixed-Metal Complexes Based on a Binuclear
 Oxovanadium Unit:&#x00A0; Synthesis, Crystal Structure, EPR, and Magnetic
 Properties
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3949
_journal_page_last               3957
_journal_paper_doi               10.1021/ic051979y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C27 H70 N6 O38 Pr V3'
_chemical_formula_weight         1380.59
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.402(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.811(7)
_cell_length_b                   20.204(7)
_cell_length_c                   26.788(10)
_cell_measurement_reflns_used    6134
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.54
_cell_volume                     10607(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35403
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.511850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         12752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+35.6107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                9149
_reflns_number_total             12752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051979ysup3.cif
_cod_data_source_block           50308f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4331983