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_4064417
_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
'2(C38 H31 Br2 N2 O2 P2 Re), 0.33 (C H2 Cl2), C4 H8 O'
_chemical_formula_sum            'C80.33 H70.67 Br4 Cl0.67 N4 O5 P4 Re2'
_chemical_formula_weight         2012.18
_chemical_name_systematic
'Acetonitrile-dibromo-(2,2'-bis(diphenylphosphino)diphenylether-P,P')-nitrosyl-rhenium(I) dichloromethane tetrahydrofuran solvate'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   44.9814(5)
_cell_length_b                   44.9814(5)
_cell_length_c                   11.4942(1)
_cell_measurement_reflns_used    19409
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.30
_cell_measurement_theta_min      2.58
_cell_volume                     20140.7(4)
_computing_cell_refinement
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction
;
CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.55
;
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 2.01.
  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 1.80.00.
 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
; Goniometer Xcalibur, detector: Ruby
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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37156
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.625
_exptl_absorpt_correction_T_max  0.622
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8838
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9889
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0526P)^2^+7.2701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                7864
_reflns_number_total             9889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200092y_si_002.cif
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4064417