Arrested α-hydride migration activates a phosphido ligand for C-H insertion.
Hickey, Anne K.; Muñoz, Salvador B; Lutz, Sean A.; Pink, Maren; Chen, Chun-Hsing; Smith, Jeremy M.; Chemical communications (Cambridge, England) 53 (2016) 412–415; doi:10.1039/c6cc07864h

data_7119195
_publ_section_title
;
 Arrested \a-hydride migration activates a phosphido ligand for C-H
 insertion.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              412
_journal_page_last               415
_journal_paper_doi               10.1039/c6cc07864h
_journal_volume                  53
_journal_year                    2016
_chemical_formula_moiety         'C48 H50 B Fe N8 P, 1.25 (C5 H12)'
_chemical_formula_sum            'C54.25 H65 B Fe N8 P'
_chemical_formula_weight         926.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3102(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1882(6)
_cell_length_b                   21.3706(8)
_cell_length_c                   29.4853(10)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.26
_cell_volume                     10035.8(6)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'0.50 degree frames measured for 20 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            180301
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.9353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G Sheldrick; 2012'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3940
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1260
_refine_ls_number_reflns         23099
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+6.6989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                17731
_reflns_number_total             23099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc07864h7.cif
_cod_data_source_block           14078
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7119195