Lanthanide Borohydride Complexes Supported by Diaminobis(phenoxide) Ligands for the Polymerization of ε-Caprolactone and l- and rac-Lactide
Fanny Bonnet; Andrew R. Cowley; Philip Mountford; Inorganic Chemistry 44 (2005) 9046–9055; doi:10.1021/ic051316g

data_4310120
_publ_contact_author
;
 Dr P. Mountford           
 Chemistry Reaearch Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
Lanthanide Borohydride Complexes Supported by Diaminobis(phenoxide) Ligands
for the Polymerization of \e-Caprolactone and l- and rac-Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9046
_journal_page_last               9055
_journal_paper_doi               10.1021/ic051316g
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C82 H110 Cl2 La2 N6 O4, 3(C6 H6) '
_chemical_formula_sum            'C100 H128 Cl2 La2 N6 O4'
_chemical_formula_weight         1826.87
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_date             31-07-05
_audit_creation_method           CRYSTALS
_cell_angle_alpha                105.7622(3)
_cell_angle_beta                 106.5123(4)
_cell_angle_gamma                90.6879(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4266(2)
_cell_length_b                   17.2972(2)
_cell_length_c                   22.1531(2)
_cell_measurement_reflns_used    20554
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     5076.90(10)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            84399
_diffrn_reflns_theta_full        27.457
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         5.148
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9678
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         17140
_refine_ls_number_restraints     340
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.039504
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.44 0.524 5.80 1.38 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0891
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0762
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              -22
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                17140
_reflns_number_total             22982
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic051316gsi20050930_121147.cif
_cod_data_source_block           COMPOUND_4-La
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:
data name '_contact_author_fax' replaced with
'_publ_contact_author_fax' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        5076.90(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C100 H128 Cl2 La2 N6 O4 '
_cod_database_code               4310120