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_4064167
_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_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C30 H42 N4 Ti1 '
_chemical_formula_sum            'C30 H42 N4 Ti'
_chemical_formula_weight         506.59
_chemical_name_systematic
; 
Cp*Ti{MeC(NiPr)2}(NNPh2)
;
_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
_cell_angle_alpha                98.8190(9)
_cell_angle_beta                 111.0632(10)
_cell_angle_gamma                104.1383(9)
_cell_formula_units_Z            2
_cell_length_a                   10.4877(2)
_cell_length_b                   11.9775(3)
_cell_length_c                   12.8157(2)
_cell_measurement_reflns_used    19244
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1404.13(5)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.045
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19244
_diffrn_reflns_theta_full        27.468
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         5.131
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' brown-green '
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0976
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001469
_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: 
 0.635 0.329 0.343 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0681
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0487
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4265
_reflns_number_total             6318
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om101167p_si_002.cif
_cod_data_source_block           compound_13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '
_cod_original_formula_sum        ' C30 H42 N4 Ti1 '
_cod_database_code               4064167