Oxidative Addition of a Diphosphine Anhydride to Iron(0) and Nickel(0): A Simple Approach to Installing Four Ligands
Ringenberg, Mark R.; Gray, Danielle L.; Rauchfuss, Thomas B.; Organometallics 30 (2011) 2885–; doi:10.1021/om200073k

data_4064390
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Oxidative Addition of a Diphosphine Anhydride to Iron(0) and Nickel(0): A
 Simple Approach to Installing Four Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2885
_journal_paper_doi               10.1021/om200073k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C40 H28 Fe O5 P2, 2(C H2 Cl2) '
_chemical_formula_sum            'C42 H32 Cl4 Fe O5 P2'
_chemical_formula_weight         876.27
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3751(11)
_cell_length_b                   19.2388(13)
_cell_length_c                   23.6101(15)
_cell_measurement_reflns_used    2788
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.46
_cell_measurement_theta_min      2.34
_cell_volume                     7892.3(9)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  fa52jas
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50391
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.9163
_exptl_absorpt_correction_T_min  0.8522
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_id                fa52jas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research)with the 2 -2 1 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7231
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+2.6281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4511
_reflns_number_total             7231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200073k_si_002.cif
_cod_data_source_block           fa52jas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               4064390