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_4064176
_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_formula_moiety         'C36 H52 N6 O2 Ti1'
_chemical_formula_sum            'C36 H52 N6 O2 Ti'
_chemical_formula_weight         648.75
_chemical_name_systematic
;
 Cp*Ti(MeDIPA){OC(NNMe2)N(Tol)C(NTol)CO}
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 102.6628(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3786(4)
_cell_length_b                   20.2596(7)
_cell_length_c                   14.3585(6)
_cell_measurement_reflns_used    7263
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3513.3(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.983
_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  0.053
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14521
_diffrn_reflns_theta_full        25.474
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         5.114
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1432
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000739
_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: 
 1.04 0.975E-01 0.758 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0743
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0486
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5111
_reflns_number_total             7609
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      9.61
_oxford_refine_ls_r_factor_ref   0.0490
_oxford_refine_ls_scale          0.3297(6)
_oxford_reflns_number_all        7609
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om101167p_si_002.cif
_cod_data_source_block           compound_35
_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        'C36 H52 N6 O2 Ti1'
_cod_database_code               4064176