Redox-Active, Boron-Based Ligands in Iron Complexes with Inverted Hydride Reactivity in Dehydrogenation Catalysis
Bäcker, Andreas; Li, Yinwu; Fritz, Maximilian; Grätz, Maik; Ke, Zhuofeng; Langer, Robert; ACS Catalysis 9 (2019) 7300–; doi:10.1021/acscatal.9b00882

data_4514651
_publ_section_title
;
 Redox-Active, Boron-Based Ligands in Iron Complexes with Inverted Hydride
 Reactivity in Dehydrogenation Catalysis
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              7300
_journal_paper_doi               10.1021/acscatal.9b00882
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C52 H46 B Fe O2 P4, 2.5(C H2 Cl2), Br'
_chemical_formula_sum            'C54.5 H51 B Br Cl5 Fe O2 P4'
_chemical_formula_weight         1185.65
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                97.02(3)
_cell_angle_beta                 94.81(3)
_cell_angle_gamma                111.71(3)
_cell_formula_units_Z            2
_cell_length_a                   11.496(2)
_cell_length_b                   12.374(3)
_cell_length_c                   20.858(4)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2709.0(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20677
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.851
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6931
_reflns_number_total             10351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b00882_si_004.cif
_cod_data_source_block           AR25b
_cod_original_cell_volume        2708.9(11)
_cod_original_formula_sum        'C54.50 H51 B Br Cl5 Fe O2 P4'
_cod_database_code               4514651
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              71177
_shelx_hkl_checksum              42946