Reactions of Cyclopentadienyl−Amidinate Titanium Hydrazides with CO2, CS2, and Isocyanates: Ti═NαCycloaddition, Cycloaddition−Insertion, and Cycloaddition−NNR2Group Transfer Reactions
Tiong, Pei Jen; Nova, Ainara; Groom, Laura R.; Schwarz, Andrew D.; Selby, Jonathan D.; Schofield, A. Daniel; Clot, Eric; Mountford, Philip; Organometallics 30 (2011) 1182–; doi:10.1021/om101167p

data_4064174
_publ_section_title
;
 Reactions of Cyclopentadienyl&#x2212;Amidinate Titanium Hydrazides with
 CO2, CS2, and Isocyanates: Ti&#x2550;N\aCycloaddition,
 Cycloaddition&#x2212;Insertion, and Cycloaddition&#x2212;NNR2Group
 Transfer Reactions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1182
_journal_paper_doi               10.1021/om101167p
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H59 N5 S1 Ti1'
_chemical_formula_sum            'C43 H59 N5 S Ti'
_chemical_formula_weight         725.94
_chemical_name_systematic
;
Cp*Ti(MeDIPA){N(NPh2)C(NAr)S}
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.13960(10)
_cell_length_b                   15.7202(2)
_cell_length_c                   21.3280(2)
_cell_measurement_reflns_used    5142
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4070.17(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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.024
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9294
_diffrn_reflns_theta_full        27.460
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         5.117
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details 'Flack (1983), 4147 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7430
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000985
_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: 
 0.925 0.590 0.697 0.163 0.162 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0630
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0494
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7880
_reflns_number_total             9269
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.11
_oxford_diffrn_Wilson_scale      5.08
_oxford_refine_ls_r_factor_ref   0.0461
_oxford_refine_ls_scale          0.4622(6)
_oxford_reflns_number_all        9269
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om101167p_si_002.cif
_cod_data_source_block           compound_29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 21 21 21 '
_cod_original_formula_sum        'C43 H59 N5 S1 Ti1'
_cod_database_code               4064174