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_1515129
_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         'C57.50 H82.50 Li2 N5.50 O0.50 Ti1'
_chemical_formula_sum            'C57.5 H82.5 Li2 N5.5 O0.5 Ti'
_chemical_formula_weight         920.61
_chemical_name_systematic
;
Ti(NAr)2(NHAr)2{Li(py)}2
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.4575(2)
_cell_length_b                   16.9731(2)
_cell_length_c                   17.7260(2)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5553.22(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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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  0.075
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12231
_diffrn_reflns_theta_full        26.944
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.28
_refine_ls_abs_structure_details 'Flack (1983), 5724 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.52(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1681
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         5838
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0006511
_refine_ls_shift/su_mean         0.0000201
_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:
0.353 0.229 0.155
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1332
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0557
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -22
_reflns_number_gt                6825
_reflns_number_total             12231
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.16
_oxford_diffrn_Wilson_scale      77.30
_oxford_refine_ls_r_factor_ref   0.0523
_oxford_refine_ls_scale          0.1326(2)
_oxford_reflns_number_all        12231
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c1sc00786f.txt
_cod_data_source_block           ads173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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 n a 21 '
_cod_original_formula_sum        'C57.50 H82.50 Li2 N5.50 O0.50 Ti1'
_cod_database_code               1515129