[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_4311183
_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 H40 As2 N3 O3 Tc'
_chemical_formula_weight         1026.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.971(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6520(9)
_cell_length_b                   16.8995(7)
_cell_length_c                   16.1837(7)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_volume                     5276.5(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34538
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         2.73
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  5.5
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.6796
_exptl_absorpt_correction_T_min  0.5273
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         15851
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                10437
_reflns_number_total             15851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049774xsi20040219_093317.cif
_cod_data_source_block           ra120603
_cod_database_code               4311183