Syntheses and characterization of phenyldiazenido and mixed phenyldiazenido‒isocyanide complexes of rhenium. Crystal structure of [ReBr2(NNPh)2(PPh3)2]
da Costa, M. Teresa A. R. S.; Dilworth, Jonathan R.; Duarte, M. Teresa; Fraústo da Silva, João J. R.; Galvão, Adelino M.; Pombeiro, Armando J. L.; Journal of the Chemical Society, Dalton Transactions  (1998) 2405–; doi:10.1039/a800898a

data_7027841
_publ_section_title
;
 Syntheses and characterization of phenyldiazenido and mixed
 phenyldiazenido--isocyanide complexes of rhenium. Crystal structure of
 [ReBr2(NNPh)2(PPh3)2]
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2405
_journal_paper_doi               10.1039/a800898a
_journal_year                    1998
_chemical_formula_sum            'C48 H40 Br2 N4 P2 Re'
_chemical_formula_weight         1080.80
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                62.020(10)
_cell_angle_beta                 91.990(10)
_cell_angle_gamma                71.550(10)
_cell_formula_units_Z            2
_cell_length_a                   12.334(2)
_cell_length_b                   12.146(3)
_cell_length_c                   17.844(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      14.2
_cell_volume                     2185.2(8)
_computing_cell_refinement       'CAD-4 software (Enraf Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf Nonius, 1989)'
_computing_data_reduction        'process-MolEN, (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4-Enraf Nonius'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5987
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0.035
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.720
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   'empirical via \y-scan North et al. (1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.885
_refine_diff_density_min         -2.368
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         5418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_obs          0.0424
_refine_ls_shift/esd_max         0.043
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+19.9248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1202
_refine_ls_wR_factor_obs         0.1134
_reflns_number_observed          5020
_reflns_number_total             5581
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a800898sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+19.9248P] 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^)+(0.0568P)^2^+19.9248P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2185.2(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027841