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_4064392
_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_absolute_configuration rm
_chemical_formula_moiety         'C41 H37 Ni O3 P3, 2 (C H2 Cl2)'
_chemical_formula_sum            'C43 H41 Cl4 Ni O3 P3'
_chemical_formula_weight         899.18
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
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_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
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_cell_length_b                   25.205(12)
_cell_length_c                   17.491(9)
_cell_measurement_reflns_used    8545
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.10
_cell_measurement_theta_min      2.27
_cell_volume                     8307(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_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       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba76iastq
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_max         20.79
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_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.9461
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_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3712
_exptl_crystal_id                ba76iastq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.102
_platon_squeeze_details
; 
The electron count from the "squeeze" model converged in fairly good agreement 
with four symmetrically independent disordered solvate molecules predicted by 
full structure refinement. 
;
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack (1983),  4123 Friedels'
_refine_ls_abs_structure_Flack   0.069(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         8646
_refine_ls_number_restraints     1637
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+5.8456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                7156
_reflns_number_total             8646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200073k_si_002.cif
_cod_data_source_block           ba76iastq
_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_H-M      'Pca2(1) '
_cod_database_code               4064392