Vanadium(iii) phenoxyimine complexes for ethylene or ε-caprolactone polymerization: mononuclear versus binuclear pre-catalysts
Clowes, Lucy; Walton, Mark; Redshaw, Carl; Chao, Yimin; Walton, Alex; Elo, Pertti; Sumerin, Victor; Hughes, David L.; Catal. Sci. Technol. 3 (2013) 152–; doi:10.1039/C2CY20571H

data_1556332
_publ_section_title
;
 Vanadium(iii) phenoxyimine complexes for ethylene or \e-caprolactone
 polymerization: mononuclear versus binuclear pre-catalysts
;
_journal_issue                   1
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              152
_journal_paper_doi               10.1039/C2CY20571H
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C38 H46 Cl2 N2 O3 V, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H52 Cl2 N4 O3 V'
_chemical_formula_weight         782.72
_chemical_name_common            'Compound 13'
_space_group_IT_number           33
_space_group_name_Hall           'P -2bc 2a'
_space_group_name_H-M_alt        'P 21 n b'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 n b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0873(5)
_cell_length_b                   17.9157(8)
_cell_length_c                   20.6832(14)
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4108.4(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971 and Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9744
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_exptl_crystal_colour            'Dark Orange'
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.8166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4516
_reflns_number_total             5871
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cy20571h.txt
_cod_data_source_block           s0481
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21nb
_cod_database_code               1556332