Preparations, Structures, and Electrochemical Studies of Aryldiazene Complexes of Rhenium: Syntheses of the First Heterobinuclear and Heterotrinuclear Derivatives with Bis(diazene) or Bis(diazenido) Bridging Ligands
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Giovanni B. Ballico; Emilio Bordignon; Giancarlo Pelizzi; Maria Ranieri; Paolo Ugo; Inorganic Chemistry 39 (2000) 3265–3279; doi:10.1021/ic991393+

data_4327648
_publ_section_title
;
 Preparations, Structures, and Electrochemical Studies of Aryldiazene
 Complexes of Rhenium: Syntheses of the First Heterobinuclear and
 Heterotrinuclear Derivatives with Bis(diazene) or Bis(diazenido) Bridging
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3265
_journal_page_last               3279
_journal_paper_doi               10.1021/ic991393+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C55 H86 B N2 O13 P4 Re'
_chemical_formula_weight         1304.15
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.33(5)
_cell_angle_beta                 91.2(1)
_cell_angle_gamma                89.71(9)
_cell_formula_units_Z            2
_cell_length_a                   15.380(5)
_cell_length_b                   13.037(5)
_cell_length_c                   16.649(5)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      9.0
_cell_volume                     3337(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\q/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19477
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.557
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         19477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                10297
_reflns_number_total             19477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9913932B.cif
_cod_data_source_block           Compound-X
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] 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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4327648