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_4312266
_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            'C29.5 H33 Cl2 N2 O0.5 P2 Re'
_chemical_formula_weight         742.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'not located'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.981(3)
_cell_length_b                   12.127(2)
_cell_length_c                   18.355(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      8.0
_cell_volume                     3098.7(11)
_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 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Siemens 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  0.0961
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9416
_diffrn_reflns_theta_full        30.34
_diffrn_reflns_theta_max         30.34
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  0.324
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.788
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0906P)^2^+16.0600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                3297
_reflns_number_total             4090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049139rsi20041011_031808.cif
_cod_data_source_block           8m.1/2(MeOH)
_cod_original_formula_sum        'C29.50 H33 Cl2 N2 O0.50 P2 Re'
_cod_database_code               4312266