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_4066539
_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         'C29 H41 N5 O4 S2 Ti1. C6 H6'
_chemical_formula_sum            'C35 H47 N5 O4 S2 Ti'
_chemical_formula_weight         713.82
_chemical_name_systematic
;
Ti{PhCH2N(CH2CH2NTs)2}(NMe2)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                 94.2902(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3514(2)
_cell_length_b                   28.2936(5)
_cell_length_c                   15.3443(3)
_cell_measurement_reflns_used    5670
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3615.56(13)
_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 0.941
_diffrn_measured_fraction_theta_max 0.935
_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  0.031
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11447
_diffrn_reflns_theta_full        26.392
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         5.096
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512.000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1309
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4788
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000919
_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: 
 0.428 -0.556 0.569E-01 -0.228 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0485
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0292
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4788
_reflns_number_total             7757
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      9.45
_oxford_refine_ls_scale          0.3402(3)
_cod_data_source_file            om100508j_si_002.cif
_cod_data_source_block           COMPOUND_19
_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/n 1 '
_cod_original_formula_sum        'C35 H47 N5 O4 S2 Ti1'
_cod_database_code               4066539