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_7222479
_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
;
C79 H111 N O7 V2, C H2 Cl2
;
_chemical_formula_sum            'C80 H113 Cl2 N O7 V2'
_chemical_formula_weight         1373.49
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-02 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                77.635(4)
_cell_angle_beta                 81.522(4)
_cell_angle_gamma                85.307(5)
_cell_formula_units_Z            1
_cell_length_a                   9.4460(6)
_cell_length_b                   11.1800(7)
_cell_length_c                   19.3754(13)
_cell_measurement_reflns_used    6954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     1974.2(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
Rigaku Kappa CCD with Saturn724+ detector.
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1230
_diffrn_reflns_av_unetI/netI     0.1748
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21387
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Implemented within Rigaku CrystalClear software. 
CrystalClear 2.1 b31
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       Plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6954
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2135
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2929
_reflns_number_total             6954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra20177b2.cif
_cod_data_source_block           6
_cod_database_code               7222479
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              48174
_shelx_hkl_checksum              21791