Coordination compounds of chromium (+3) and vanadium (+3) and (+5) with 2,6-bis(diphenylhydroxymethyl)pyridyl ligand: Synthesis and study of catalytic activity in the polymerization of ethylene
Dmitry A. Kurmaev; Nicolai A. Kolosov; Svetlana Ch. Gagieva; Alexandra O. Borissova; Vladislav A. Tuskaev; Natalya M. Bravaya; Boris M. Bulychev; Inorganica Chimica Acta 396 (2013) 136–143; doi:10.1016/j.ica.2012.11.006

data_1513011
_publ_section_title
;
 Coordination compounds of chromium (+3) and vanadium (+3) and (+5) with
 2,6-bis(diphenylhydroxymethyl)pyridyl ligand: Synthesis and study of
 catalytic activity in the polymerization of ethylene
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              136
_journal_page_last               143
_journal_paper_doi               10.1016/j.ica.2012.11.006
_journal_volume                  396
_journal_year                    2013
_chemical_formula_moiety         'C31 H23 Cl N O3 V'
_chemical_formula_sum            'C31 H23 Cl N O3 V'
_chemical_formula_weight         543.89
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.386(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5834(10)
_cell_length_b                   15.1756(10)
_cell_length_c                   16.0379(12)
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2515.9(3)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14763
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9484
_exptl_absorpt_correction_T_min  0.9398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1546
_reflns_number_gt                4766
_reflns_number_total             6610
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ICA-2013-396-136-143-4.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1513011