Iron-57 NMR and Structural Study of [Fe(η5-Cp)(SnPh3)(CO)(PR3)] (PR3= Phosphine, Phosphite). Separation of Steric and Electronic σ and π Effects
Mampa, Richard M.; Fernandes, Manuel A.; Carlton, Laurence; Organometallics  (2014) 140626113119005–; doi:10.1021/om4011593

data_4083765
_publ_section_title
;
 Iron-57 NMR and Structural Study of [Fe(\h5-Cp)(SnPh3)(CO)(PR3)] (PR3=
 Phosphine, Phosphite). Separation of Steric and Electronic \s and \p
 Effects
;
_journal_name_full               Organometallics
_journal_page_first              140626113119005
_journal_paper_doi               10.1021/om4011593
_journal_year                    2014
_chemical_formula_moiety         'C45 H32 F9 Fe O P Sn'
_chemical_formula_sum            'C45 H32 F9 Fe O P Sn'
_chemical_formula_weight         965.22
_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
_cell_angle_alpha                74.464(2)
_cell_angle_beta                 83.455(2)
_cell_angle_gamma                62.597(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5624(3)
_cell_length_b                   11.8279(4)
_cell_length_c                   16.6985(6)
_cell_measurement_reflns_used    6033
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.19
_cell_volume                     1953.23(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21434
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.9150
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Face indexed absorption correction carried out with XPREP
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7669
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.6187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                5251
_reflns_number_total             7669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4011593_si_002.cif
_cod_data_source_block           12m_rm6_0a-cmpd11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1953.23(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083765