Synthesis of Zwitterionic Triphosphenium Transition Metal Complexes: A Boron Atom Makes The Difference
Jonathan W. Dube; Charles L. B. Macdonald; Bobby D. Ellis; Paul J. Ragogna; Inorganic Chemistry 52 (2013) 11438–11449; doi:10.1021/ic401766j

data_4336274
_publ_contact_author_address
;1151 Richmond Street
London
Ontario
Canada
N6A 5B7
;
_publ_contact_author_email       pragogna@uwo.ca
_publ_contact_author_fax         1-519-661-3022
_publ_contact_author_name        'Prof. Paul J. Ragogna'
_publ_contact_author_phone       '519-661-2111 ex 87048'
_publ_section_title
;
 Synthesis of Zwitterionic Triphosphenium Transition Metal Complexes: A
 Boron Atom Makes The Difference
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11438
_journal_page_last               11449
_journal_paper_doi               10.1021/ic401766j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H34 B Fe O4 P3, C4 H10 O'
_chemical_formula_sum            'C46 H44 B Fe O5 P3'
_chemical_formula_weight         836.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.905(10)
_cell_length_b                   9.3403(16)
_cell_length_c                   21.160(4)
_cell_measurement_reflns_used    9447
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.79
_cell_volume                     8282(3)
_computing_cell_refinement       SAINT
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  cif_to_tables
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1147
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            124931
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0459P)^2^+8.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                6699
_reflns_number_total             9869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401766j_si_002_5.cif
_cod_data_source_block           2Fe
_cod_database_code               4336274