Family of Mixed-Valence Oxovanadium(IV/V) Dinuclear Entities Incorporating N4O3-Coordinating Heptadentate Ligands: Synthesis, Structure, and EPR Spectra
Amrita Mondal; Sumana Sarkar; Deepak Chopra; T. N. Guru Row; Kausikisankar Pramanik; Kajal Krishna Rajak; Inorganic Chemistry 44 (2005) 703–708; doi:10.1021/ic048919x

data_4308475
_publ_contact_author_address
;
Department of Chemistry, Inorganic Chemistry Section,
Jadavpur University, Kolkata 700 032, India.
;
_publ_contact_author_email       kajalrajak@hotmail.com
_publ_contact_author_name        'Dr. Kajal K. Rajak'
_publ_section_title
;
Family of Mixed-Valence Oxovanadium(IV/V) Dinuclear Entities Incorporating
N4O3-Coordinating Heptadentate Ligands: Synthesis, Structure, and EPR
Spectra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              703
_journal_page_last               708
_journal_paper_doi               10.1021/ic048919x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C32 H43 Cl2 N4 O6 V2'
_chemical_formula_weight         752.48
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.461(4)
_cell_length_b                   17.230(3)
_cell_length_c                   13.700(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.50
_cell_volume                     3851.9(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.1359
_diffrn_reflns_av_sigmaI/netI    0.1748
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6304
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.8616
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrik, 1997'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       parallopiped
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.958
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.1936
_refine_ls_R_factor_obs          0.1020
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1751P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3472
_refine_ls_wR_factor_obs         0.2568
_reflns_number_observed          1419
_reflns_number_total             2989
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic048919xsi20040806_105016.cif
_cod_data_source_block           V2O3L1.CH2Cl2
_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 2.4.1 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1751P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1751P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3852.0(13)
_cod_database_code               4308475