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_7027326
_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_sum            'C93 H102 B F24 N2 O3 P2 Re'
_chemical_formula_weight         2010.79
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             98-04-07
_audit_creation_method           CRYSTALS
_cell_angle_alpha                97.76(2)
_cell_angle_beta                 107.96(2)
_cell_angle_gamma                102.88(2)
_cell_formula_units_Z            2
_cell_length_a                   13.892(3)
_cell_length_b                   18.768(3)
_cell_length_c                   19.569(3)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    153
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     4615.8(17)
_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)                                                            
 SCHAKAL (Keller, 1992)                                                         
;
_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
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_diffrn_ambient_temperature      153
_diffrn_measurement_device       ' Siemens P4 '
_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 Ka'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_refln_scan_mode          om
_diffrn_refln_scan_width         1.6
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16842
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.46
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             2046.04
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   0.9612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         15223
_refine_ls_R_factor_obs          0.0539
_refine_ls_shift/esd_max         0.011569
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;                                                                               
 Chebychev polynomial (Carruthers & Watkin, 1979)                               
;
_refine_ls_wR_factor_obs         0.0385
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_observed          15223
_reflns_number_total             16060
_reflns_observed_criterion       >0.00s(I)
_cod_data_source_file            901384isup1.cif
_cod_data_source_block           IV+
_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        4615.77
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C93.00 H102.00 Re1 P2 F24.00 O3 N2 B1 '
_cod_database_code               7027326