Ring-opening polymerization of ε-caprolactone by lithium piperazinyl-aminephenolate complexes: synthesis, characterization and kinetic studies.
Ikpo, Nduka; Hoffmann, Christian; Dawe, Louise N.; Kerton, Francesca M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 6651–6660; doi:10.1039/c2dt30276d

data_7019149
_publ_section_title
;
 Ring-opening polymerization of \e-caprolactone by lithium
 piperazinyl-aminephenolate complexes: synthesis, characterization and
 kinetic studies.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6651
_journal_page_last               6660
_journal_paper_doi               10.1039/c2dt30276d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C66 H111 Li3 N6 O3'
_chemical_formula_sum            'C66 H111 Li3 N6 O3'
_chemical_formula_weight         1057.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.574(3)
_cell_angle_beta                 103.944(5)
_cell_angle_gamma                90.860(4)
_cell_formula_units_Z            2
_cell_length_a                   9.905(2)
_cell_length_b                   18.234(5)
_cell_length_c                   20.026(6)
_cell_measurement_reflns_used    13077
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.5914
_cell_measurement_theta_min      2.2634
_cell_volume                     3331.3(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32540
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.9879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         13769
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.1008
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+1.5404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2768
_refine_ls_wR_factor_ref         0.2940
_reflns_number_gt                11046
_reflns_number_total             13769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30276d.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3331.4(15)
_cod_database_code               7019149