Formation of an iron phosphine-borane complex by formal insertion of BH₃ into the Fe-P bond.
Frank, Nicolas; Hanau, Katharina; Flosdorf, Kimon; Langer, Robert; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11252–11261; doi:10.1039/c3dt51254a

data_7023383
_publ_section_title
;
 Formation of an iron phosphine-borane complex by formal insertion of
 BH&#x2083; into the Fe-P bond.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11252
_journal_page_last               11261
_journal_paper_doi               10.1039/c3dt51254a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C52 H48 Fe N4 P4, Cl4 Fe, C2 H3 N '
_chemical_formula_sum            'C54 H51 Cl4 Fe2 N5 P4'
_chemical_formula_weight         1147.38
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.401(5)
_cell_length_b                   12.421(3)
_cell_length_c                   19.403(4)
_cell_measurement_reflns_used    61659
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.1
_cell_measurement_theta_min      1.81
_cell_volume                     5399(2)
_computing_cell_refinement       'X-Area 1.56 (Stoe 2011)'
_computing_data_collection       'X-Area 1.56 (Stoe 2011)'
_computing_data_reduction        'X-Area 1.56 (Stoe 2011)'
_computing_molecular_graphics    'DIAMOND 3.2g (Brandenburg 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE Stadi Vari'
_diffrn_measurement_method       omega-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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69797
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.9158
_exptl_absorpt_correction_T_min  0.8413
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Stoe, X-Area Ver. 1.56'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         16368
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                11420
_reflns_number_total             16368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51254a.txt
_cod_data_source_block           Compound2
_cod_original_cell_volume        5398.7(19)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7023383