[TcI(CN)3(CO)3]2- and [ReI(CN)3(CO)3]2-: Case Studies for the Binding Properties of CN- and CO
Philipp Kurz; Bernhard Spingler; Thomas Fox; Roger Alberto; Inorganic Chemistry 43 (2004) 3789–3791; doi:10.1021/ic049774x

data_4311184
_publ_section_title
;
 [TcI(CN)3(CO)3]2- and [ReI(CN)3(CO)3]2-: Case Studies for the Binding
 Properties of CN- and CO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3789
_journal_page_last               3791
_journal_paper_doi               10.1021/ic049774x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C54 H48 As2 N3 O7 Re'
_chemical_formula_weight         1186.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.991(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5656(4)
_cell_length_b                   13.1567(5)
_cell_length_c                   41.3637(19)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_volume                     5204.9(4)
_computing_cell_refinement       'IPDS (Stoe,1999)'
_computing_data_collection       'IPDS (Stoe,1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation scan'
_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  0.1056
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            34613
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.63
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  28
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  0.9102
_exptl_absorpt_correction_T_min  0.5038
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         12559
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                6602
_reflns_number_total             12559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049774xsi20040219_093331.cif
_cod_data_source_block           pk070403
_cod_database_code               4311184