Co-ordination chemistry of the [Re(NO)2(PR3)2]+ fragment: crystallographic and computational studies †
Jacobsen, Heiko; Heinze, Katja; Llamazares, Angela; Schmalle, Helmut W.; Artus, Georg; Berke, Heinz; Journal of the Chemical Society, Dalton Transactions  (1999) 1717–; doi:10.1039/a901384i

data_7027327
_publ_section_title
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 Co-ordination chemistry of the [Re(NO)2(PR3)2]+ fragment:
 crystallographic and computational studies&#x200A;&#x2020;
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_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1717
_journal_paper_doi               10.1039/a901384i
_journal_year                    1999
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C36 H85 N4 O4 P4 Re2 1+, C32 H12 B1 F24 1-'
_chemical_formula_sum            'C68 H97 B F24 N4 O4 P4'
_chemical_formula_weight         1997.61
_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_date             98-03-16
_audit_creation_method           CRYSTALS
_cell_angle_alpha                97.22(1)
_cell_angle_beta                 93.87(1)
_cell_angle_gamma                96.11(1)
_cell_formula_units_Z            2.00
_cell_length_a                   14.256(2)
_cell_length_b                   16.859(2)
_cell_length_c                   17.771(2)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    183(5)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      10.9
_cell_volume                     4199.0(9)
_computing_cell_refinement       'Siemens P3/PC Diffractometer Program'
_computing_data_collection       'Siemens P3/PC Diffractometer Program'
_computing_data_reduction
;                                                                               
 SHELXTL PLUS Package (Siemens 1994) and                                        
 CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)               
;
_computing_molecular_graphics
;                                                                               
 PLATON (Spek, 1995)                                                            
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      183(5)
_diffrn_measurement_device       ' Siemens P3 '
_diffrn_measurement_method
;                                                                               
 omega scan, variable scan speed from 2 to 29deg/min                            
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_refln_scan_mode          omega
_diffrn_refln_scan_width         1.2
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15368
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        9.40
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.09
_exptl_absorpt_correction_T_max  0.394
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '6 reflections with \c > 80 \%'
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         7.68
_refine_diff_density_min         -3.58
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.1395
_refine_ls_hydrogen_treatment
;
 Depending on the disordering the hydrogen atoms positions were
 either calculated once and refined as rigid group together with the
 neighbouring carbon atom or the hydrogens were calculated after every
 cycle.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         10254
_refine_ls_R_factor_obs          0.1104
_refine_ls_shift/esd_max         0.001166
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;                                                                               
 Chebychev polynomial (Carruthers & Watkin, 1979)                               
;
_refine_ls_wR_factor_obs         0.0813
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_observed          10254
_reflns_number_total             14579
_reflns_observed_criterion       >1.00s(I)
_cod_data_source_file            901384isup1.cif
_cod_data_source_block           V+
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4198.9(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C68 H97 B1 F24 N4 O4 P4 '
_cod_database_code               7027327