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_4336214
_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            'C54.5 H63 Cl2 N4 O2 Ta'
_chemical_formula_weight         1057.94
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                108.9610(10)
_cell_angle_beta                 101.4700(10)
_cell_angle_gamma                91.2710(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9766(7)
_cell_length_b                   13.0697(9)
_cell_length_c                   19.1327(13)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.31
_cell_volume                     2532.8(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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25586
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    2.319
_exptl_absorpt_correction_T_max  0.8920
_exptl_absorpt_correction_T_min  0.5806
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         9282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+2.0837P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8482
_reflns_number_total             9282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401496w_si_002_5.cif
_cod_data_source_block           afh358
_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_original_formula_sum        'C54.50 H63 Cl2 N4 O2 Ta'
_cod_database_code               4336214
_shelx_estimated_absorpt_t_min   0.515
_shelx_estimated_absorpt_t_max   0.851
_shelxl_version_number           2013-2
_shelx_res_checksum              90111