Early Transition Metal Complexes Containing 1,2,4-Triazolato and Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
Carlos Yélamos; Karl R. Gust; Anwar G. Baboul; Mary Jane Heeg; H. Bernhard Schlegel; Charles H. Winter; Inorganic Chemistry 40 (2001) 6451–6462; doi:10.1021/ic0109389

data_4320677
_publ_section_title
;
 Early Transition Metal Complexes Containing 1,2,4-Triazolato and
 Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6451
_journal_page_last               6462
_journal_paper_doi               10.1021/ic0109389
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H50 N10 Ti'
_chemical_formula_weight         598.70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 121.6160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   33.981(2)
_cell_length_b                   16.2356(8)
_cell_length_c                   23.0511(11)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     10829.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELX-97
_computing_structure_refinement  SHELX-97
_computing_structure_solution    SHELX-97
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.054
_diffrn_reflns_av_sigmaI/netI    0.081
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.910
_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11475
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_refine_ls_restrained_S_obs      1.045
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_refine_ls_R_factor_obs          0.0555
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_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1676
_refine_ls_wR_factor_obs         0.1366
_reflns_number_observed          6085
_reflns_number_total             11478
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0109389_1.cif
_cod_data_source_block           pztz(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10829.9(9)
_cod_database_code               4320677