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_4336276
_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
'C43 H34 B Cr O5 P3, 0.68(C3 Cr O), 0.32(C H2 Cl2)'
_chemical_formula_sum            'C45.36 H34.64 B Cl0.64 Cr1.68 O7.05 P3'
_chemical_formula_weight         905.6
_chemical_name_systematic
; 
 ? 
;
_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                101.638(16)
_cell_angle_beta                 91.474(12)
_cell_angle_gamma                114.719(15)
_cell_formula_units_Z            2
_cell_length_a                   9.940(4)
_cell_length_b                   10.936(5)
_cell_length_c                   22.352(10)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.27
_cell_volume                     2145.1(17)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57290
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             927
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0000P)^2^+6.3724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                7310
_reflns_number_total             9819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401766j_si_002_7.cif
_cod_data_source_block           3Cr
_cod_original_cell_volume        2145.1(16)
_cod_original_formula_sum        'C45.36 H34.64 B1 Cl0.64 Cr1.68 O7.05 P3'
_cod_database_code               4336276