Synthesis and structures of titanium and yttrium complexes with N,N′-tetramethylguanidinate ligands: different reactivity of the M‒N bonds toward phenyl isocyanate
Zhang, Jie; Han, Fuyan; Han, Yanan; Chen, Zhenxia; Zhou, Xigeng; Dalton Transactions  (2009) 1806–1811; doi:10.1039/b817776g

data_7000680
_publ_section_title
;
 Synthesis and structures of titanium and yttrium complexes with
 N,N&#x2032;-tetramethylguanidinate ligands: different reactivity of
 the M--N bonds toward phenyl isocyanate
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1806
_journal_page_last               1811
_journal_paper_doi               10.1039/b817776g
_journal_year                    2009
_chemical_formula_sum            'C15 H22 Cl N3 Ti'
_chemical_formula_weight         327.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.595(4)
_cell_length_b                   15.297(4)
_cell_length_c                   15.395(4)
_cell_measurement_reflns_used    872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.511
_cell_measurement_theta_min      2.974
_cell_volume                     3201.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13972
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        4.63
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9337
_exptl_absorpt_correction_T_min  0.8453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+1.8995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                1981
_reflns_number_total             3153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817776g.txt
_cod_data_source_block           f50329b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3201.7(14)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7000680