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_4331982
_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 H66 Ce N6 O36 V3'
_chemical_formula_weight         1343.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                61.892(2)
_cell_angle_beta                 83.132(3)
_cell_angle_gamma                89.212(2)
_cell_formula_units_Z            2
_cell_length_a                   13.799(3)
_cell_length_b                   14.070(3)
_cell_length_c                   14.693(3)
_cell_measurement_reflns_used    4702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.31
_cell_volume                     2495.2(9)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'APEX II 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
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_diffrn_reflns_av_R_equivalents  0.0185
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_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13294
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.669030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1370
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_exptl_crystal_size_min          0.20
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_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^)+(0.0693P)^2^+0.0692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                7014
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051979ysup2.cif
_cod_data_source_block           50304f
_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 2.4.2 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2495.1(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331982