Reactivity of hydride bridges in a high-spin [Fe3(μ-H)3]3+ cluster: reversible H2/CO exchange and Fe‒H/B‒F bond metathesis
Anderton, Kevin J.; Knight, Brian J.; Rheingold, Arnold L.; Abboud, Khalil A.; García-Serres, Ricardo; Murray, Leslie J.; Chem. Sci.  (2017) –; doi:10.1039/C6SC05583D

data_1545736
_publ_section_title
;
 Reactivity of hydride bridges in a high-spin [Fe3(\m-H)3]3+ cluster:
 reversible H2/CO exchange and Fe--H/B--F bond metathesis
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC05583D
_journal_year                    2017
_chemical_formula_sum            'C59 H76 Fe3 N6 O2'
_chemical_formula_weight         1068.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-21 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                77.1659(11)
_cell_angle_beta                 87.1605(10)
_cell_angle_gamma                84.1531(11)
_cell_formula_units_Z            2
_cell_length_a                   12.5204(6)
_cell_length_b                   13.0808(7)
_cell_length_c                   16.5376(8)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     2626.1(2)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex2 SAINT (Bruker, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/7, Sheldrick, G. M. 2014'
_computing_structure_refinement  'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_structure_solution    'SHELXL2014/7, Sheldrick G. M. 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50075
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.263
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.8105
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         12038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.1907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9908
_reflns_number_total             12038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05583d2.cif
_cod_data_source_block           kand16
_cod_database_code               1545736
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              82821