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_4083760
_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 H41 Fe O P Sn, 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H45 Cl4 Fe O P Sn'
_chemical_formula_weight         973.14
_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                 111.1140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6443(4)
_cell_length_b                   11.0577(2)
_cell_length_c                   20.4132(4)
_cell_measurement_reflns_used    8104
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.41
_cell_volume                     4347.05(15)
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33542
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7492
_exptl_absorpt_correction_T_min  0.6398
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Face indexed absorption corrections carried out with XPREP
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                8104
_reflns_number_total             10481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4011593_si_002.cif
_cod_data_source_block           12m_rm4_0a-cmpd6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        4347.05(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4083760