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_7027325
_publ_section_title
;
 Co-ordination chemistry of the [Re(NO)2(PR3)2]+ fragment:
 crystallographic and computational studies&#x200A;&#x2020;
;
_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_formula_sum            'C69.5 H79 B Cl F24 N2 O3 P2 Re'
_chemical_formula_weight         1740.75
_chemical_name_systematic
; 
 Bis(tricyclohexylphosphine)carbonyldinitrosylrhenium(-I) 
 Tetrakis(3,5-bis(trifluoromethyl)phenyl)borate
;
_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-97
_cell_angle_alpha                79.633(12)
_cell_angle_beta                 71.952(11)
_cell_angle_gamma                79.440(11)
_cell_formula_units_Z            2
_cell_length_a                   12.9909(12)
_cell_length_b                   16.6700(16)
_cell_length_c                   19.0701(19)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.3
_cell_volume                     3826.4(7)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'STOE IPDS diffractometer'
_diffrn_measurement_method       'phi rotation scan mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48209
_diffrn_reflns_theta_full        30.30
_diffrn_reflns_theta_max         30.30
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.5686
_exptl_absorpt_correction_T_min  0.3928
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         3.045
_refine_diff_density_min         -5.186
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0105(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         20707
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.389
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                15863
_reflns_number_total             20707
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            901384isup1.cif
_cod_data_source_block           III+
_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.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' 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        3826.4(6)
_cod_original_formula_sum        'C69.50 H79 B Cl F24 N2 O3 P2 Re'
_cod_database_code               7027325