Tuning the Electronic and Steric Parameters of a Redox-Active Tris(amido) Ligand
Rui F. Munhá; Ryan A. Zarkesh; Alan F. Heyduk; Inorganic Chemistry 52 (2013) 11244–11255; doi:10.1021/ic401496w

data_4336215
_publ_section_title
;
 Tuning the Electronic and Steric Parameters of a Redox-Active Tris(amido)
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11244
_journal_page_last               11255
_journal_paper_doi               10.1021/ic401496w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C26 H32 Cl2 N3 Ta'
_chemical_formula_weight         638.39
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8131(6)
_cell_length_b                   10.6877(6)
_cell_length_c                   23.9902(14)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.55
_cell_volume                     2516.1(3)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26584
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.368
_diffrn_reflns_theta_min         1.698
_exptl_absorpt_coefficient_mu    4.600
_exptl_absorpt_correction_T_max  0.3014
_exptl_absorpt_correction_T_min  0.1955
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+4.6828P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2625
_reflns_number_total             2789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401496w_si_002_6.cif
_cod_data_source_block           afh370
_cod_depositor_comments
;
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 
;
_cod_database_code               4336215
_shelx_estimated_absorpt_t_min   0.287
_shelx_estimated_absorpt_t_max   0.365
_shelxl_version_number           2013-2
_shelx_res_checksum              9243