Rhenium Nitrosyl Complexes Bearing Large-Bite-Angle Diphosphines
Dudle, Balz; Rajesh, Kunjanpillai; Blacque, Olivier; Berke, Heinz; Organometallics 30 (2011) 2986–; doi:10.1021/om200092y

data_4064416
_publ_section_title
;
 Rhenium Nitrosyl Complexes Bearing Large-Bite-Angle Diphosphines
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2986
_journal_paper_doi               10.1021/om200092y
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H31 Br2 Fe N2 O P2 Re, C4 H8 O'
_chemical_formula_sum            'C40 H39 Br2 Fe N2 O2 P2 Re'
_chemical_formula_weight         1043.53
_chemical_name_systematic
'Acetonitrile-dibromo-(1,1'-bis(diphenylphosphino)ferrocene-P,P')-nitrosyl-rhenium(I) tetrahydrofuran monosolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.971(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9650(1)
_cell_length_b                   32.0257(4)
_cell_length_c                   12.1774(2)
_cell_measurement_reflns_used    17453
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.64
_cell_measurement_theta_min      2.43
_cell_volume                     3827.55(9)
_computing_cell_refinement
;
CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24
;
_computing_data_collection
;
CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24
;
_computing_data_reduction
;
CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24
;
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 1.08.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX - An integrated system of Windows programs for the solution,
 refinment and analysis of single crystal X-ray diffraction data,
 Version 1.70.01.
 Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97. Program for crystal structure refinement.
 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows, Version 1.12.
 Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Oxford Diffraction (2007). Oxford Diffraction Ltd., 
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38549
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    5.748
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
R.C. Clark and J.S. Reid, Acta Cryst. 1995, A51, 887-897
implemented in the CrysAlis Software system, Oxford Diffraction Ltd.,
Version 1.171.32.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         11676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                8661
_reflns_number_total             11676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200092y_si_002.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064416