Ring-opening polymerization of rac-lactide mediated by tetrametallic lithium and sodium diamino-bis(phenolate) complexes.
Alhashmialameer, Dalal; Ikpo, Nduka; Collins, Julie; Dawe, Louise N.; Hattenhauer, Karen; Kerton, Francesca M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20216–20231; doi:10.1039/c5dt03119b

data_7037096
_publ_section_title
;
 Ring-opening polymerization of rac-lactide mediated by tetrametallic
 lithium and sodium diamino-bis(phenolate) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20216
_journal_page_last               20231
_journal_paper_doi               10.1039/c5dt03119b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C82 H132 Li4 N4 O7, 3(C7H8)'
_chemical_formula_sum            'C103 H156 Li4 N4 O7'
_chemical_formula_weight         1590.15
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    Moisture-sensitive
_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
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                103.219(7)
_cell_angle_beta                 98.581(7)
_cell_angle_gamma                109.095(8)
_cell_formula_units_Z            2
_cell_length_a                   16.592(2)
_cell_length_b                   18.655(2)
_cell_length_c                   19.067(2)
_cell_measurement_reflns_used    26644
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.0
_cell_volume                     5265.8(11)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'FS-PROCESS (Rigaku, 2009)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_solution    'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43063
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 119 electrons per 
unit cell in two voids (total volume 813 ^A^3); that is 59.5 electrons 
per formula unit. Disordered lattice solvent toluene  molecules 
(50 electrons per C7H8; 1 molecule per formula unit) were present 
prior to the application of Squeeze, however, a satisfactory 
point atom model could not be achieved.  Note that there are two 
well-ordered toluene molecules associated with each formula unit that 
were not removed using Squeeze. The application of Squeeze gave 
a good improvement in the data statistics and allowed for a 
full anisotropic refinement of the  structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         21429
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.1130
_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^)+(0.1609P)^2^+12.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3441
_refine_ls_wR_factor_ref         0.3597
_reflns_number_gt                13730
_reflns_number_total             21429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03119b2.cif
_cod_data_source_block           IN0162
_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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7037096--7037097.cif.
;
_cod_original_cell_volume        5265.8(10)
_cod_database_code               7037096