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_7023386
_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         'C50 H46 Fe N3 P4, C2 H3 N, B H4'
_chemical_formula_sum            'C52 H53 B Fe N4 P4'
_chemical_formula_weight         924.52
_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                102.39(3)
_cell_angle_beta                 93.89(3)
_cell_angle_gamma                106.63(3)
_cell_formula_units_Z            4
_cell_length_a                   13.018(3)
_cell_length_b                   19.641(4)
_cell_length_c                   20.451(4)
_cell_measurement_reflns_used    20573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.613
_cell_volume                     4847(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      ' 208 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.1428
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37872
_diffrn_reflns_theta_full        26.20
_diffrn_reflns_theta_max         26.20
_diffrn_reflns_theta_min         1.32
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           32
_diffrn_source_power             1.60
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.9028
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-Red32 1.53'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         19049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                10514
_reflns_number_total             19049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51254a.txt
_cod_data_source_block           rl210b
_cod_original_cell_volume        4846.7(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7023386