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_4064172
_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         'C27 H40 N4 O4 Ti1'
_chemical_formula_sum            'C27 H40 N4 O4 Ti'
_chemical_formula_weight         532.54
_chemical_name_systematic
;
Cp*Ti(MeDIPA){OC(O)N(NMePh)C(O)O}
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 112.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9970(5)
_cell_length_b                   16.9143(9)
_cell_length_c                   9.8429(5)
_cell_measurement_reflns_used    3081
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1383.05(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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 0.990
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       Area
_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  0.070
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7564
_diffrn_reflns_theta_full        26.154
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         5.146
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details 'Flack (1983), 2737 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       170(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1081
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.0001020
_refine_ls_shift/su_mean         0.0000080
_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: 
 0.623 -0.388 0.384 -0.149 0.621E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0915
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0529
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                4077
_reflns_number_total             5983
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0562
_oxford_refine_ls_scale          0.3950(10)
_oxford_reflns_number_all        5983
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om101167p_si_002.cif
_cod_data_source_block           compound_36
_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_cell_volume        1383.06(13)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C27 H40 N4 O4 Ti1'
_cod_database_code               4064172