The Crucial Role of the Diphosphine Heteroatom X in the Stereochemistry and Stabilization of the Substitution-Inert [M(N)(PXP)]2+ Metal Fragments (M = Tc, Re; PXP = Diphosphine Ligand)
Francesco Tisato; Fiorenzo Refosco; Marina Porchia; Cristina Bolzati; Giuliano Bandoli; Alessandro Dolmella; Adriano Duatti; Alessandra Boschi; Christian M. Jung; Hans-Juergen Pietzsch; Werner Kraus; Inorganic Chemistry 43 (2004) 8617–8625; doi:10.1021/ic049139r

data_4312264
_publ_section_title
;
 The Crucial Role of the Diphosphine Heteroatom X in the Stereochemistry
 and Stabilization of the Substitution-Inert [M(N)(PXP)]2+ Metal Fragments
 (M = Tc, Re; PXP = Diphosphine Ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8617
_journal_page_last               8625
_journal_paper_doi               10.1021/ic049139r
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C29 H31 Cl4 N2 P2 Tc'
_chemical_formula_weight         709.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.65(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.310(2)
_cell_length_b                   17.708(3)
_cell_length_c                   15.197(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      7.5
_cell_volume                     3119.8(9)
_computing_cell_refinement       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_computing_publication_material  'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nicolet R3m/V diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5485
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00000(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          1.741
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                3753
_reflns_number_total             5485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049139rsi20040701_071623.cif
_cod_data_source_block           1.CH2Cl2
_cod_original_cell_volume        3119.8(8)
_cod_database_code               4312264