Ring-Opening Polymerization ofrac-Lactide by Bis(phenolate)amine-Supported Samarium Borohydride Complexes: An Experimental and DFT Study
Dyer, Hellen E.; Huijser, Saskia; Susperregui, Nicolas; Bonnet, Fanny; Schwarz, Andrew D.; Duchateau, Robbert; Maron, Laurent; Mountford, Philip; Organometallics 29 (2010) 3602–; doi:10.1021/om100513j

data_4066553
_publ_section_title
;
 Ring-Opening Polymerization ofrac-Lactide by
 Bis(phenolate)amine-Supported Samarium Borohydride Complexes: An
 Experimental and DFT Study
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3602
_journal_paper_doi               10.1021/om100513j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C41 H73 N2 O4 Si2 Sm1, C5H12'
_chemical_formula_sum            'C46 H85 N2 O4 Si2 Sm'
_chemical_formula_weight         936.76
_chemical_name_systematic
;
Sm(O2N_OMe){N(SiHMe2)2}(THF)
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.7826(11)
_cell_angle_beta                 98.6551(11)
_cell_angle_gamma                101.7293(8)
_cell_formula_units_Z            2
_cell_length_a                   11.2380(2)
_cell_length_b                   15.4597(3)
_cell_length_c                   15.9220(3)
_cell_measurement_reflns_used    34435
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2629.19(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius (1997-2001). COLLECT.'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34435
_diffrn_reflns_theta_full        25.232
_diffrn_reflns_theta_max         27.426
_diffrn_reflns_theta_min         5.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8772
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001863
_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: 
 0.481 0.682E-01 0.204 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0534
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0374
_refine_special_details
;
The SiH hydrogen atoms were located in a difference Fourier map and their 
coordinates and isotropic displacement parameters subsequently refined. 
Other hydrogen atoms were positioned geometrically.

The large displacement parameters of the solvent suggest that it may be 
disordered. It was not possible to resolve two or more sites for any of its 
atoms or to model the disorder.
;
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -20
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8772
_reflns_number_total             11833
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2358(2)
_cod_data_source_file            om100513j_si_002.cif
_cod_data_source_block           COMPOUND_7
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C46 H85 N2 O4 Si2 Sm1'
_cod_database_code               4066553