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_4066543
_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
'C71 H67 F36.00 N8 O12 S6 Si2 Zr2, 3.5(C6 H6)'
_chemical_formula_sum            'C92 H88 F36 N8 O12 S6 Si2 Zr2'
_chemical_formula_weight         2612.69
_chemical_name_systematic
;
[Zr(N3ArFN)(CH2SiMe3)]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_method           CRYSTALS_ver_12.86
_cell_angle_alpha                64.3587(5)
_cell_angle_beta                 88.4433(5)
_cell_angle_gamma                84.7710(5)
_cell_formula_units_Z            2
_cell_length_a                   17.7133(2)
_cell_length_b                   18.3479(2)
_cell_length_c                   18.5380(2)
_cell_measurement_reflns_used    22052
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5408.45(11)
_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 0.987
_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  0.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42232
_diffrn_reflns_theta_full        26.688
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         5.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.91
_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            colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2639.999
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.70
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1531
_refine_ls_number_reflns         14445
_refine_ls_number_restraints     304
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.104276
_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: 
 0.892 0.244 0.662 0.554E-01 0.171 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0918
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0595
_reflns_limit_h_max              23
_reflns_limit_h_min              -22
_reflns_limit_k_max              23
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                16190
_reflns_number_total             24559
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.02
_oxford_diffrn_Wilson_scale      35.19
_oxford_refine_ls_r_factor_ref   0.0549
_oxford_refine_ls_scale          0.16714(19)
_oxford_reflns_number_all        24559
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om100508j_si_002.cif
_cod_data_source_block           COMPOUND_32
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C92 H88 F36.00 N8 O12 S6 Si2 Zr2'
_cod_database_code               4066543