Reactions of a Cyclopentadienyl–Amidinate Titanium Benzimidamido Complex
Groom, Laura R.; Russell, Adam F.; Schwarz, Andrew D.; Mountford, Philip; Organometallics 33 (2014) 1002–; doi:10.1021/om4011752

data_4082403
_publ_section_title
;
 Reactions of a Cyclopentadienyl--Amidinate Titanium Benzimidamido Complex
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1002
_journal_paper_doi               10.1021/om4011752
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C14 H16 F5 N3 O1'
_chemical_formula_sum            'C14 H16 F5 N3 O'
_chemical_formula_weight         337.29
_chemical_name_systematic
;
Me2NC(NC(C6F5)NOtBu)H 
;
_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     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.3332(11)
_cell_angle_beta                 110.0682(12)
_cell_angle_gamma                102.2578(9)
_cell_formula_units_Z            2
_cell_length_a                   8.3723(2)
_cell_length_b                   8.6069(2)
_cell_length_c                   12.1306(2)
_cell_measurement_reflns_used    2818
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     779.42(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.961
_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  0.016
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5747
_diffrn_reflns_theta_full        26.345
_diffrn_reflns_theta_max         27.732
_diffrn_reflns_theta_min         5.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_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            yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.0003652
_refine_ls_shift/su_mean         0.0000291
_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: 
 1.00 0.176 0.681 0.378E-01 0.175 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0454
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0367
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                2864
_reflns_number_total             3515
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.67
_oxford_diffrn_Wilson_scale      0.32
_oxford_refine_ls_r_factor_ref   0.0353
_oxford_refine_ls_scale          1.805(3)
_oxford_reflns_number_all        3515
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om4011752_si_002.cif
_cod_data_source_block           compound_16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C14 H16 F5 N3 O1'
_cod_database_code               4082403