Ethylene Reactions of a [ReH(η2-BH4)(NO)(PPh3)2] Complex: Reductive Elimination of Ethane and Oxidative Coupling to Butadiene
Dudle, Balz; Blacque, Olivier; Berke, Heinz; Organometallics 31 (2012) 1832–; doi:10.1021/om201187w

data_4076416
_publ_section_title
;
 Ethylene Reactions of a [ReH(\h2-BH4)(NO)(PPh3)2] Complex: Reductive
 Elimination of Ethane and Oxidative Coupling to Butadiene
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1832
_journal_paper_doi               10.1021/om201187w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H25 N O P Re'
_chemical_formula_sum            'C24 H25 N O P Re'
_chemical_formula_weight         560.63
_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                 104.302(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0774(2)
_cell_length_b                   22.2969(5)
_cell_length_c                   10.8304(3)
_cell_measurement_reflns_used    13823
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.68
_cell_measurement_theta_min      2.66
_cell_volume                     2124.11(9)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 1997) and/or <i>Mercury</i> (Macrae et
al., 2006)
;
_computing_publication_material
; 
<i>WinGX</i> (Farrugia, 1999), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_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  'Xcalibur, Ruby'
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27820
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.810
_exptl_absorpt_correction_T_max  0.278
_exptl_absorpt_correction_T_min  0.102
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.35.11 (Agilent Technologies, 2011)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid (1995).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.842
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0208P)^2^+2.1788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                5985
_reflns_number_total             6483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201187w_si_001.cif
_cod_data_source_block           4ph
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076416