Vanadium(V) tetra-phenolate complexes: Synthesis, structural studies and ethylene homo-(co-)polymerization capability
Redshaw, Carl; Walton, Mark; Elsegood, Mark Robert James; Prior, Timothy J.; Michiue, Kenji; RSC Adv.  (2015) –; doi:10.1039/C5RA20177B

data_7222477
_publ_section_title
;
 Vanadium(V) tetra-phenolate complexes: Synthesis, structural studies and
 ethylene homo-(co-)polymerization capability
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA20177B
_journal_year                    2015
_chemical_formula_moiety
;
C78 H116 O10 V2, 2(C4 H8 O)
;
_chemical_formula_sum            'C86 H132 O12 V2'
_chemical_formula_weight         1459.80
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-02 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8164(16)
_cell_length_b                   18.9585(7)
_cell_length_c                   18.6002(6)
_cell_measurement_reflns_used    34672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      3.0
_cell_measurement_theta_min      27.5
_cell_volume                     8398.4(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Shldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57655
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
A multi-scan absorption correction was implemented
within Rigaku CrystalClear. 

Tmax = 1; Tmin = 0.511
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         9280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                5352
_reflns_number_total             9280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra20177b2.cif
_cod_data_source_block           1
_cod_database_code               7222477