Ligand Variations in New Sulfonamide-Supported Group 4 Ring-Opening Polymerization Catalysts
Schwarz, Andrew D.; Herbert, Katherine R.; Paniagua, Cristina; Mountford, Philip; Organometallics 29 (2010) 4171–; doi:10.1021/om100508j

data_4066542
_publ_section_title
;
 Ligand Variations in New Sulfonamide-Supported Group 4 Ring-Opening
 Polymerization Catalysts
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4171
_journal_paper_doi               10.1021/om100508j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C62 H88 N8 O12 S6 Si2 Zr2, 2(C6 H6)'
_chemical_formula_sum            'C74 H100 N8 O12 S6 Si2 Zr2'
_chemical_formula_weight         1724.66
_chemical_name_systematic
;
[Zr(CH2SiMe3){(N(Ts)CH2CH2)3N}]2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 112.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.120(2)
_cell_length_b                   32.411(7)
_cell_length_c                   12.042(2)
_cell_measurement_reflns_used    7708
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      5.097
_cell_volume                     4021.8(16)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15361
_diffrn_reflns_theta_full        25.197
_diffrn_reflns_theta_max         27.094
_diffrn_reflns_theta_min         5.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0798
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6533
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001726
_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: 
 0.692 0.725E-01 0.345 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0449
_refine_ls_wR_factor_gt          0.0338
_refine_ls_wR_factor_ref         0.0338
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              41
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                6533
_reflns_number_total             8572
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      10.24
_oxford_refine_ls_scale          0.3312(3)
_cod_data_source_file            om100508j_si_002.cif
_cod_data_source_block           COMPOUND_30
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4021.7(16)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4066542