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_1513009
_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         'C124 H94 Cr2 N4 O8, (C7 H8), (C4 H8 O)'
_chemical_formula_sum            'C135 H110 Cr2 N4 O9'
_chemical_formula_weight         2036.27
_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
_cell_angle_alpha                103.0380(10)
_cell_angle_beta                 98.8750(10)
_cell_angle_gamma                96.7890(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7934(5)
_cell_length_b                   12.8886(5)
_cell_length_c                   16.6146(7)
_cell_measurement_reflns_used    2351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2603.45(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31409
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         13822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                8976
_reflns_number_total             13822
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ICA-2013-396-136-143-2.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513009