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_4083768
_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         '2(C42 H35 Fe O4 P Sn), C7 H8'
_chemical_formula_sum            'C91 H78 Fe2 O8 P2 Sn2'
_chemical_formula_weight         1710.55
_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                102.302(2)
_cell_angle_beta                 103.441(3)
_cell_angle_gamma                93.486(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9203(13)
_cell_length_b                   10.1167(13)
_cell_length_c                   20.665(3)
_cell_measurement_reflns_used    893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.91
_cell_measurement_theta_min      2.53
_cell_volume                     1957.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11641
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.8986
_exptl_absorpt_correction_T_min  0.8112
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Face indexed absorption correction carried out with XPREP
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismic
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7609
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.4945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                6322
_reflns_number_total             7609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4011593_si_002.cif
_cod_data_source_block           4m_lc6_a-cmpd14
_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        1957.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083768