Structural and Electronic Comparison of 1st Row Transition Metal Complexes of a Tripodal Iminopyridine Ligand
Ashley M. McDaniel; Anthony K. Rappé; Matthew P. Shores; Inorganic Chemistry 51 (2012) 12493–12502; doi:10.1021/ic301909u

data_4331094
_publ_section_title
;
 Structural and Electronic Comparison of 1st Row Transition Metal
 Complexes of a Tripodal Iminopyridine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12493
_journal_page_last               12502
_journal_paper_doi               10.1021/ic301909u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H33 F6 N7 O12 S2 Zn'
_chemical_formula_weight         951.14
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Bruker SHELXTL'
_audit_update_record
;
2012-01-31 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.042(2)
_cell_length_b                   10.042(2)
_cell_length_c                   35.268(9)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.41
_cell_volume                     3080.0(12)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19212
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plates
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2979
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                2735
_reflns_number_total             2979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301909u_si_002_6.cif
_cod_data_source_block           msn301
_cod_original_cell_volume        3079.8(12)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4331094
_publcif_info_exptl_table_max_cols 6