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_7119194
_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 H48 B1 Fe1 N8 P1'
_chemical_formula_sum            'C48 H48 B Fe N8 P'
_chemical_formula_weight         834.59
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-03-23
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                106.3844(10)
_cell_angle_beta                 90.0628(11)
_cell_angle_gamma                91.3197(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2416(5)
_cell_length_b                   12.4664(5)
_cell_length_c                   13.9258(6)
_cell_measurement_reflns_used    4974
_cell_measurement_temperature    100
_cell_measurement_theta_max      16
_cell_measurement_theta_min      2
_cell_volume                     2038.29(15)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11548
_diffrn_reflns_theta_full        12.697
_diffrn_reflns_theta_max         16.929
_diffrn_reflns_theta_min         0.990
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.32
_refine_diff_density_min         -1.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1659
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         11517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.0046983
_refine_ls_shift/su_mean         0.0000599
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 3.35P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1774
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1771
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7464
_reflns_number_total             11548
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.13
_oxford_diffrn_Wilson_scale      15.25
_oxford_refine_ls_r_factor_ref   0.1119
_oxford_refine_ls_scale          0.2586(2)
_oxford_reflns_number_all        11521
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'cmc1056_0m in P-1'
_cod_data_source_file            c6cc07864h7.cif
_cod_data_source_block           S16004
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C48 H48 B1 Fe1 N8 P1'
_cod_database_code               7119194