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_4082195
_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_formula_moiety         'C46 H68 N4 O2 Ti2'
_chemical_formula_sum            'C46 H68 N4 O2 Ti2'
_chemical_formula_weight         804.87
_chemical_name_systematic
;
[Cp*Ti{PhC(NiPr)2}(mu-O)]2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 110.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.088(6)
_cell_length_b                   10.816(2)
_cell_length_c                   26.575(5)
_cell_measurement_reflns_used    20475
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8625(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            37605
_diffrn_reflns_theta_full        26.931
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0811
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         12385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0007140
_refine_ls_shift/su_mean         0.0000258
_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: 
 0.961 0.706 0.577 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0867
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0564
_reflns_limit_h_max              38
_reflns_limit_h_min              -41
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                13687
_reflns_number_total             19606
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      29.38
_oxford_refine_ls_r_factor_ref   0.0468
_oxford_refine_ls_scale          0.1887(2)
_oxford_reflns_number_all        19606
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om401008a_si_002.cif
_cod_data_source_block           compound_23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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/c '
_cod_database_code               4082195