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_4066541
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H42 N4 O5 S2 Ti1'
_chemical_formula_sum            'C30 H42 N4 O5 S2 Ti'
_chemical_formula_weight         650.72
_chemical_melting_point
; 
No special details
;
_chemical_name_systematic
;
Ti{PhCH2N(CH2CH2NTs)2}(NMe2)(OiPr)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                90
_cell_angle_beta                 102.4530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.38760(10)
_cell_length_b                   18.7925(3)
_cell_length_c                   10.4541(2)
_cell_measurement_reflns_used    3653
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1609.05(4)
_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 0.988
_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       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5838
_diffrn_reflns_theta_full        26.114
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         5.095
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.43
_refine_ls_abs_structure_details 'Flack (1983), 2070 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000198
_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: 
 0.687 0.225 0.355 0.715E-01 0.147E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0425
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0358
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -24
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                5436
_reflns_number_total             5829
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.63
_oxford_diffrn_Wilson_scale      2.59
_oxford_refine_ls_r_factor_ref   0.0328
_oxford_refine_ls_scale          0.6427(7)
_oxford_reflns_number_all        5829
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om100508j_si_002.cif
_cod_data_source_block           COMPOUND_24
_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_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C30 H42 N4 O5 S2 Ti1'
_cod_database_code               4066541