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_4064391
_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         'C58 H28 B F15 Fe O5 P2'
_chemical_formula_sum            'C58 H28 B F15 Fe O5 P2'
_chemical_formula_weight         1218.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.069(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6244(9)
_cell_length_b                   17.9336(11)
_cell_length_c                   22.4793(14)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.83
_cell_measurement_theta_min      2.15
_cell_volume                     6236.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1762
_diffrn_reflns_av_sigmaI/netI    0.1308
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            96818
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9594
_exptl_absorpt_correction_T_min  0.8786
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_id                ba72jasq
_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 1 2 scattering 

planes roughly normal to the spindle axis. 

;
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.102
_platon_squeeze_details
;
The positions of the dichloromethane solvate molecules were poorly resolved
so their electron density contribution to the data was removed with the 
BYPASS proceedure in Platon, squeeze.  The electron density removed is
consistent with the 3 symmetrically independent solvate molecules being present 
4 times each within the unit cell.
;
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         11499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                6115
_reflns_number_total             11499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200073k_si_002.cif
_cod_data_source_block           ba72jasq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064391