Diazo Complexes of Rhenium: Preparations and Crystal Structures of the Bis(dinitrogen), [Re(N2)2{PPh(OEt)2}4][BPh4] and Methyldiazenido [ReCl(CH3N2)(CH3NHNH2){PPh(OEt)2}3][BPh4] Derivatives
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Emilio Bordignon; Francesca Miani; Giancarlo Pelizzi; Inorganic Chemistry 39 (2000) 3283–3293; doi:10.1021/ic990970r

data_4321178
_publ_section_title
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 Diazo Complexes of Rhenium: Preparations and Crystal Structures of the
 Bis(dinitrogen), [Re(N2)2{PPh(OEt)2}4][BPh4] and Methyldiazenido
 [ReCl(CH3N2)(CH3NHNH2){PPh(OEt)2}3][BPh4] Derivatives
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3283
_journal_page_last               3293
_journal_paper_doi               10.1021/ic990970r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C64 H80 B N4 O8 P4 Re'
_chemical_formula_weight         1354.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2b'
_symmetry_space_group_name_H-M   'P b a a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.008(5)
_cell_length_b                   23.367(5)
_cell_length_c                   12.863(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.41
_cell_measurement_theta_min      4.78
_cell_volume                     6916(3)
_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 .918
_diffrn_measured_fraction_theta_max .918
_diffrn_measurement_device_type  'Philips PW100 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  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19904
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        25
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .442
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2784
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.652
_refine_diff_density_rms         .098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         10103
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3846
_reflns_number_total             10103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990970r_1.cif
_cod_data_source_block           Compound_[Re(N2)2{PPh(OEt)2}4]BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'othorhombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^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^)+(0.0513P)^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 
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_cod_original_formula_sum        'C64 H80 B1 N4 O8 P4 Re1'
_cod_database_code               4321178