Sulfonamide-Supported Group 4 Catalysts for the Ring-Opening Polymerization of ε-Caprolactone and rac-Lactide
Andrew D. Schwarz; Amber L. Thompson; Philip Mountford; Inorganic Chemistry 48 (2009) 10442–10454; doi:10.1021/ic901524s

data_4303513
_publ_contact_author
;
 Prof P. Mountford           
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
Sulfonamide-Supported Group 4 Catalysts for the Ring-Opening Polymerization
of \e-Caprolactone and rac-Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10442
_journal_page_last               10454
_journal_paper_doi               10.1021/ic901524s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C27 H43 N3 O7 S2 Zr1'
_chemical_formula_sum            'C27 H43 N3 O7 S2 Zr'
_chemical_formula_weight         677.01
_chemical_name_systematic
;
Zr(L_OMe)(OiPr)2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             08-09-08
_cell_angle_alpha                90
_cell_angle_beta                 92.7258(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.01950(10)
_cell_length_b                   9.89890(10)
_cell_length_c                   31.5596(4)
_cell_measurement_reflns_used    7267
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3126.60(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            13761
_diffrn_reflns_theta_full        26.942
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         5.151
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_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: 
 0.653 0.471 0.579 0.197 0.155 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0554
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0355
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                5183
_reflns_number_total             7099
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.94
_oxford_diffrn_Wilson_scale      38.32
_oxford_refine_ls_r_factor_ref   0.0376
_oxford_refine_ls_scale          0.1743(2)
_oxford_reflns_number_all        7099
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic901524s_si_001_1.cif
_cod_data_source_block           COMPOUND_15
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C27 H43 N3 O7 S2 Zr1'
_cod_database_code               4303513