C2-Symmetric Iron(II) Diphosphine‒Dialkoxide Dicarbonyl and Related Complexes
Lei, Hao; Royer, Aaron M.; Rauchfuss, Thomas B.; Gray, Danielle; Organometallics 31 (2012) 6408–; doi:10.1021/om300631a

data_4079272
_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
;
 C2-Symmetric Iron(II) Diphosphine--Dialkoxide Dicarbonyl and Related
 Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6408
_journal_paper_doi               10.1021/om300631a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C40 H30 B2 F6 Fe O4 P2, 2(C D2 Cl2)'
_chemical_formula_sum            'C42 H28 B2 Cl4 D6 F6 Fe O4 P2'
_chemical_formula_weight         1003.94
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                67.817(3)
_cell_angle_beta                 76.915(4)
_cell_angle_gamma                83.142(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9085(8)
_cell_length_b                   12.9178(9)
_cell_length_c                   15.5436(10)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.40
_cell_volume                     2155.1(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  ba01las
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30332
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.7913
_exptl_absorpt_correction_T_min  0.7224
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_id                ba01las
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.577
_exptl_crystal_size_mid          0.573
_exptl_crystal_size_min          0.433
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7896
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0766P)^2^+5.5832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                6431
_reflns_number_total             7896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300631a_si_002.cif
_cod_data_source_block           ba01las
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4079272