Excited-State Characteristics of Tetracyanidonitridorhenium(V) and -technetium(V) Complexes with N-Heteroaromatic Ligands
Hayato Ikeda; Akitaka Ito; Eri Sakuda; Noboru Kitamura; Tsutomu Takayama; Tsutomu Sekine; Atsushi Shinohara; Takashi Yoshimura; Inorganic Chemistry 52 (2013) 6319–6327; doi:10.1021/ic302463v

data_4334995
_publ_section_title
;
 Excited-State Characteristics of Tetracyanidonitridorhenium(V) and
 -technetium(V) Complexes with N-Heteroaromatic Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6319
_journal_page_last               6327
_journal_paper_doi               10.1021/ic302463v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C65 H53 Cl4 N6 P2 Re'
_chemical_formula_sum            'C65 H53 Cl4 N6 P2 Re'
_chemical_formula_weight         1308.14
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.8025(18)
_cell_length_b                   13.3672(14)
_cell_length_c                   25.167(4)
_cell_measurement_reflns_used    48209
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.05
_cell_volume                     5989.0(13)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56928
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2632.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.930
_refine_diff_density_min         -1.370
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6698 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.591(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13709
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1474P)^2^+28.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2556
_reflns_number_gt                10936
_reflns_number_total             13709
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic302463v_si_002_04.cif
_cod_data_source_block           (PPh4)2[ReN(CN)4(ppy)]
_cod_original_cell_volume        5989.1(12)
_cod_database_code               4334995