Steric and Electronic Consequences of Flexibility in a Tetradentate Redox-Active Ligand: Ti(IV) and Zr(IV) Complexes
Géza Szigethy; Alan F. Heyduk; Inorganic Chemistry 50 (2011) 125–135; doi:10.1021/ic101468p

data_4324092
_publ_section_title
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 Steric and Electronic Consequences of Flexibility in a Tetradentate
 Redox-Active Ligand: Ti(IV) and Zr(IV) Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              125
_journal_page_last               135
_journal_paper_doi               10.1021/ic101468p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C18 H32 N10 O2 Ti'
_chemical_formula_sum            'C18 H32 N10 O2 Ti'
_chemical_formula_weight         468.44
_chemical_name_common            (N2N2)Ti(N3)2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.3700(10)
_cell_angle_beta                 76.5230(10)
_cell_angle_gamma                72.1880(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6998(7)
_cell_length_b                   10.7251(7)
_cell_length_c                   11.5990(8)
_cell_measurement_reflns_used    6259
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.56
_cell_volume                     1111.16(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      152(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13392
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.96290
_exptl_absorpt_correction_T_min  0.89262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0433P)^2^+1.0968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                4196
_reflns_number_total             5302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101468p_si_002_3.cif
_cod_data_source_block           afh221
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4324092