An anionic phosphenium complex as an ambident nucleophile.
Stadelmann, B.; Bender, J.; Förster, D; Frey, W.; Nieger, M.; Gudat, D.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6023–6031; doi:10.1039/c5dt00008d

data_7033993
_publ_section_title
;
 An anionic phosphenium complex as an ambident nucleophile.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6023
_journal_page_last               6031
_journal_paper_doi               10.1039/c5dt00008d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C29 H36 Fe N2 O3 P, C24 H20 P, 1.5 (C4 H8 O)'
_chemical_formula_sum            'C59 H68 Fe N2 O4.5 P2'
_chemical_formula_weight         994.94
_chemical_melting_point_gt       623.15
_chemical_name_systematic
'tetraphenylphosphonium {1,3-bis-(2,6-diisopropylphenyl)-1,3,2-diazaphospholenium}-tricarbonyl ferrate(II)'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-03 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.0086(16)
_cell_length_b                   12.8494(10)
_cell_length_c                   43.849(3)
_cell_measurement_reflns_used    13642
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      3.01
_cell_volume                     10710.1(14)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_molecular_graphics    'SHELXS, plus XP (Sheldrick, 1991)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            56223
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (sheldrick, 2008, cf. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             4224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofurane'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.473(15)
_refine_ls_extinction_coef       0.00085(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1231
_refine_ls_number_reflns         18565
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0353P)^2^+3.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                13658
_reflns_number_total             18565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00008d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>350C' was changed to
'623.15' - it was converted from degrees Celsius(C) to Kelvins(K).

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7033990--7033994.cif.
;
_cod_original_cell_volume        10710.2(14)
_cod_original_formula_sum        'C59 H68 Fe N2 O4.50 P2'
_cod_database_code               7033993