C3 Symmetric vanadium(III) complexes with O,N-chelating hexadentate tripodal ligands of pyrazolone
Jadeja, Rajendrasinh; Parihar, Sanjay; Gupta, Vivek; RSC Adv.  (2014) –; doi:10.1039/C4RA04021J

data_7218099
_publ_section_title
;
 C3 Symmetric vanadium(III) complexes with O,N-chelating hexadentate
 tripodal ligands of pyrazolone
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA04021J
_journal_year                    2014
_chemical_formula_moiety         'C42 H48 N10 O3'
_chemical_formula_sum            'C42 H48 N10 O3'
_chemical_formula_weight         740.90
_chemical_name_systematic
;
(4Z,4'E,4"E)-4,4',4"-(((nitrilotris(ethane-2,1-diyl)tris
(azanediyl))tris(methanylylidene))tris(3-methyl-1-(p-tolyl)-
1H-pyrazol-5(4H)-one
;
_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                65.299(4)
_cell_angle_beta                 89.444(5)
_cell_angle_gamma                84.799(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5266(5)
_cell_length_b                   13.6775(7)
_cell_length_c                   14.9717(6)
_cell_measurement_reflns_used    4975
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0473
_cell_measurement_theta_min      3.5144
_cell_volume                     1949.35(17)
_computing_cell_refinement       'SAINT 6.45 (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  PLATON(Spek,2009)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14834
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.98800
_exptl_absorpt_correction_T_min  0.98020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2003'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0096(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                3811
_reflns_number_total             7623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra04021j2.cif
_cod_data_source_block           sj143
_cod_original_cell_volume        1949.35(16)
_cod_database_code               7218099