Disubstituted 1,8-Diamidonaphthalene Ligands as a Flexible, Responsive, and Reactive Framework for Tantalum Complexes
Nathalie Lavoie; Serge I. Gorelsky; Zhixian Liu; Tara J. Burchell; Glenn P. A. Yap; Darrin S. Richeson; Inorganic Chemistry 49 (2010) 5231–5240; doi:10.1021/ic1003963

data_4315668
_publ_section_title
;
 Disubstituted 1,8-Diamidonaphthalene Ligands as a Flexible, Responsive,
 and Reactive Framework for Tantalum Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5231
_journal_page_last               5240
_journal_paper_doi               10.1021/ic1003963
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H16 Cl3 N2 Ta, 0.5(C6 H14)'
_chemical_formula_sum            'C25 H23 Cl3 N2 Ta'
_chemical_formula_weight         638.75
_chemical_name_systematic
;
 ?
;
_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                70.028(7)
_cell_angle_beta                 85.467(7)
_cell_angle_gamma                78.172(7)
_cell_formula_units_Z            2
_cell_length_a                   7.907(5)
_cell_length_b                   12.406(8)
_cell_length_c                   13.806(9)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     1245.8(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      203(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.889
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4528
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    4.748
_exptl_absorpt_correction_T_max  0.7890
_exptl_absorpt_correction_T_min  0.4300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Void space analysis consistent with initial solutions
showing one half-occupied, severely disordered hexane 
solvate per compound molecule.
 
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2918
_reflns_number_total             4528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003963_si_002_1.cif
_cod_data_source_block           dr2016s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1245.7(14)
_cod_database_code               4315668