peri-Substituted Phosphino-Phosphonium Salts: Synthesis and Reactivity
Ray, Matthew J.; Slawin, Alexandra M. Z.; Bühl, Michael; Kilian, Petr; Organometallics 32 (2013) 3481–; doi:10.1021/om400259h

data_4089477
_publ_section_title
;
 peri-Substituted Phosphino-Phosphonium Salts: Synthesis and Reactivity
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3481
_journal_paper_doi               10.1021/om400259h
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C29 H32.50 Cl Fe N0.50 P2'
_chemical_formula_sum            'C29 H32.5 Cl Fe N0.5 P2'
_chemical_formula_weight         541.33
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.657(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.505(2)
_cell_length_b                   19.460(5)
_cell_length_c                   18.170(5)
_cell_measurement_reflns_used    7807
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.25
_cell_volume                     2648.3(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16595
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nEEDLE
_exptl_crystal_F_000             1132.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0604P)^2^+2.0871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                3609
_reflns_number_total             4807
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400259h_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        2648.4(12)
_cod_original_formula_sum        'C29 H32.50 Cl Fe N0.50 P2'
_cod_database_code               4089477