Chelated Hydrazido(3-)rhenium(V) Complexes: On the Way to the Nitrido-M(V) Core (M = Tc, Re)
Franck Mévellec; Nicolas Lepareur; Alain Roucoux; Nicolas Noiret; Henri Patin; Giuliano Bandoli; Marina Porchia; Francesco Tisato; Inorganic Chemistry 41 (2002) 1591–1597; doi:10.1021/ic0110979

data_4317738
_publ_section_title
;
 Chelated Hydrazido(3-)rhenium(V) Complexes: On the Way to the
 Nitrido-M(V) Core (M = Tc, Re)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1591
_journal_page_last               1597
_journal_paper_doi               10.1021/ic0110979
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C38 H33 Cl2 N2 P2 Re S2'
_chemical_formula_weight         900.82
_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   no
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.514(4)
_cell_length_b                   10.639(2)
_cell_length_c                   20.106(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      7.7
_cell_volume                     3660.5(14)
_computing_cell_refinement       'Philips PW1100-FEBO system'
_computing_data_collection       'Philips PW1100-FEBO system'
_computing_data_reduction        'Philips PW1100-FEBO system'
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       theta-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  0.0016
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3921
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.63
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 180
_diffrn_standards_number         three
_exptl_absorpt_coefficient_mu    3.697
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   'empirical psi-scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(13)
_refine_ls_extinction_coef       0.00000(8)
_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   1.089
_refine_ls_hydrogen_treatment    no
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          3.116
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+36.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3879
_reflns_number_total             3919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110979_2.cif
_cod_data_source_block           renio_compound3
_cod_original_cell_volume        3660.5(13)
_cod_database_code               4317738