Vanadyl phenolate complexes for ring opening homo- and co-polymerisation of epsilon-caprolactone, L-lactide and rac-lactide
Ge, Feijie; Dan, Yi; Al-Khafaji, Yahya; Prior, Timothy J.; Jiang, Long; Elsegood, Mark Robert James; Redshaw, Carl; RSC Adv.  (2015) –; doi:10.1039/C5RA24816G

data_7223604
_publ_section_title
;
 Vanadyl phenolate complexes for ring opening homo- and co-polymerisation
 of &#xF065;epsilon-caprolactone, L-lactide and rac-lactide
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA24816G
_journal_year                    2015
_chemical_formula_moiety         'C71 H102 O8 V2, 3(C H2 Cl2)'
_chemical_formula_sum            'C74 H108 Cl6 O8 V2'
_chemical_formula_weight         1440.18
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-02 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.682(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.479(15)
_cell_length_b                   14.382(9)
_cell_length_c                   25.952(18)
_cell_measurement_reflns_used    10927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.7
_cell_volume                     7789(9)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1961
_diffrn_reflns_av_unetI/netI     0.1227
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50396
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.315
_diffrn_source                   'DLS Station I19'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 ? 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11066
_refine_ls_number_restraints     701
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_gt           0.1279
_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^)+(0.1902P)^2^+15.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3218
_refine_ls_wR_factor_ref         0.3700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6500
_reflns_number_total             11066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra24816g2.cif
_cod_data_source_block           5_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7223604
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              35232
_shelx_fab_checksum              57993