Synthesis and Characterization of Rhenium(III) and Technetium(III) Organohydrazide Chelate Complexes. Reactions of 2-Hydrazinopyridine with Complexes of Rhenium and Technetium
Melissa Hirsch-Kuchma; Terrence Nicholson; Alan Davison; William M. Davis; Alun G. Jones; Inorganic Chemistry 36 (1997) 3237–3241; doi:10.1021/ic961489t

data_4323504
_publ_section_title
;
 Synthesis and Characterization of Rhenium(III) and Technetium(III)
 Organohydrazide Chelate Complexes. Reactions of 2-Hydrazinopyridine with
 Complexes of Rhenium and Technetium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3237
_journal_page_last               3241
_journal_paper_doi               10.1021/ic961489t
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C41.5 H34 Cl2 N3 O0.5 P2 Re'
_chemical_formula_weight         901.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.9050(10)
_cell_angle_beta                 95.8930(10)
_cell_angle_gamma                111.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5549(7)
_cell_length_b                   12.2699(8)
_cell_length_c                   16.8206(12)
_cell_measurement_temperature    188(2)
_cell_volume                     1906.1(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7684
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_T_max  0.6355
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.959
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.0082(9)
_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_all   1.223
_refine_ls_goodness_of_fit_obs   1.179
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.319
_refine_ls_restrained_S_obs      1.179
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.022
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+9.5106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1713
_refine_ls_wR_factor_obs         0.1454
_reflns_number_observed          4792
_reflns_number_total             5273
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961489t_1.cif
_cod_data_source_block           copy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+9.5106P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+9.5106P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C41.50 H34 Cl2 N3 O0.50 P2 Re'
_cod_database_code               4323504