The first group 4 metal bis(imido) and tris(imido) complexes
Schwarz, Andrew D.; Nielson, Alastair J.; Kaltsoyannis, Nikolas; Mountford, Philip; Chemical Science 3 (2012) 819–; doi:10.1039/c1sc00786f

data_1515128
_publ_section_title
;
 The first group 4 metal bis(imido) and tris(imido) complexes
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              819
_journal_paper_doi               10.1039/c1sc00786f
_journal_volume                  3
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H69 Li3 N6 Ti1'
_chemical_formula_sum            'C52 H69 Li3 N6 Ti'
_chemical_formula_weight         846.88
_chemical_name_systematic
;
Ti(Me)(NAr)3{Li(py)}3
;
_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                 101.982(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2991(7)
_cell_length_b                   19.4178(12)
_cell_length_c                   13.0747(9)
_cell_measurement_reflns_used    5019
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     2557.8(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 0.988
_diffrn_measured_fraction_theta_max 0.986
_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  0.065
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27191
_diffrn_reflns_theta_full        25.496
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         5.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details 'Flack (1983), 2291 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.0004448
_refine_ls_shift/su_mean         0.0000162
_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:
1.54 0.226E-01 1.24
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0841
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0493
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                6557
_reflns_number_total             9570
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.88
_oxford_diffrn_Wilson_scale      4.52
_oxford_refine_ls_r_factor_ref   0.0555
_oxford_refine_ls_scale          0.5016(8)
_oxford_reflns_number_all        9570
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c1sc00786f.txt
_cod_data_source_block           ADS168
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 21 1 '
_cod_original_formula_sum        'C52 H69 Li3 N6 Ti1'
_cod_database_code               1515128