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_4303519
_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         'C30 H42 N4 O6 S2 Zr1'
_chemical_formula_sum            'C30 H42 N4 O6 S2 Zr'
_chemical_formula_weight         710.04
_chemical_name_systematic
;
Zr(L_py)(OiPr)2 
;
_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
_audit_creation_date             07-06-15
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                85.4348(14)
_cell_angle_beta                 78.1548(15)
_cell_angle_gamma                84.6582(16)
_cell_formula_units_Z            2
_cell_length_a                   9.2206(2)
_cell_length_b                   9.6331(2)
_cell_length_c                   18.7269(5)
_cell_measurement_reflns_used    13210
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1617.76(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.986
_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  0.028
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12541
_diffrn_reflns_theta_full        25.260
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.94
_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            'light brown'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0757
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.000375
_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: 
 0.461 0.207 0.223 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0504
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0370
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5477
_reflns_number_total             7284
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.02
_oxford_diffrn_Wilson_scale      11.88
_cod_data_source_file            ic901524s_si_001_7.cif
_cod_data_source_block           COMPOUND_14
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C30 H42 N4 O6 S2 Zr1'
_cod_database_code               4303519