Synthesis and Reactions of a Cyclopentadienyl-Amidinate Titaniumtert-Butoxyimido Compound
Groom, Laura R.; Schwarz, Andrew D.; Nova, Ainara; Clot, Eric; Mountford, Philip; Organometallics 32 (2013) 7520–; doi:10.1021/om401008a

data_4082193
_publ_section_title
;
 Synthesis and Reactions of a Cyclopentadienyl-Amidinate
 Titaniumtert-Butoxyimido Compound
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7520
_journal_paper_doi               10.1021/om401008a
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H43 N3 O1 Ti1'
_chemical_formula_sum            'C27 H43 N3 O Ti'
_chemical_formula_weight         473.51
_chemical_name_systematic
;
C5Me5Ti(PhDIPA)(NOtBu)
;
_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            8
_cell_length_a                   16.6135(2)
_cell_length_b                   17.1813(2)
_cell_length_c                   19.3943(2)
_cell_measurement_reflns_used    6909
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5535.94(11)
_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 0.990
_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  0.0389
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65185
_diffrn_reflns_theta_full        26.929
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.28
_refine_ls_abs_structure_details 'Flack (1983), 5711 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.52(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0998
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7629
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.0005598
_refine_ls_shift/su_mean         0.0000220
_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: 
 0.381 0.228 0.172 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1035
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0520
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8647
_reflns_number_total             12594
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.50
_oxford_diffrn_Wilson_scale      40.04
_oxford_refine_ls_r_factor_ref   0.0459
_oxford_refine_ls_scale          0.1573(2)
_oxford_reflns_number_all        12594
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om401008a_si_002.cif
_cod_data_source_block           compound_19
_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 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C27 H43 N3 O1 Ti1'
_cod_database_code               4082193