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_4082199
_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         'C13 H21 N2, C24 H20 B1'
_chemical_formula_sum            'C37 H41 B N2'
_chemical_formula_weight         524.56
_chemical_name_systematic
;
[PhC{N(iPr)H}2][BPh4]
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.985(6)
_cell_angle_beta                 105.885(6)
_cell_angle_gamma                95.944(6)
_cell_formula_units_Z            2
_cell_length_a                   9.7572(8)
_cell_length_b                   10.1086(7)
_cell_length_c                   16.5470(11)
_cell_measurement_reflns_used    4544
_cell_measurement_temperature    150
_cell_measurement_theta_max      66
_cell_measurement_theta_min      4
_cell_volume                     1532.0(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.975
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13322
_diffrn_reflns_theta_full        66.280
_diffrn_reflns_theta_max         66.190
_diffrn_reflns_theta_min         4.482
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1459
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3559
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.0029477
_refine_ls_shift/su_mean         0.0001875
_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: 
 35.9 18.9 34.2 16.4 2.19 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0314
_refine_ls_wR_factor_gt          0.0284
_refine_ls_wR_factor_ref         0.0284
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3559
_reflns_number_total             5117
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.71
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0581
_oxford_refine_ls_scale          6.016(11)
_oxford_reflns_number_all        5094
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            om401008a_si_002.cif
_cod_data_source_block           compound_33-BPh4
_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 2.4.2 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 -1 '
_cod_original_formula_sum        'C37 H41 B1 N2'
_cod_database_code               4082199