Iron Complex-Catalyzed Ammonia-Borane Dehydrogenation. A Potential Route toward B-N-Containing Polymer Motifs Using Earth-Abundant Metal Catalysts
R. Tom Baker; John C. Gordon; Charles W. Hamilton; Neil J. Henson; Po-Heng Lin; Steven Maguire; Muralee Murugesu; Brian L. Scott; Nathan C. Smythe; Journal of the American Chemical Society 134 (2012) 5598–5609; doi:10.1021/ja210542r

data_4117730
_publ_section_title
;
 Iron Complex-Catalyzed Ammonia-Borane Dehydrogenation. A Potential Route
 toward B-N-Containing Polymer Motifs Using Earth-Abundant Metal Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5598
_journal_page_last               5609
_journal_paper_doi               10.1021/ja210542r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C40 H62 Fe N2 P2'
_chemical_formula_weight         688.71
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.697(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.443(13)
_cell_length_b                   20.06(2)
_cell_length_c                   16.304(19)
_cell_measurement_temperature    140(1)
_cell_volume                     3689(7)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w 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  0.2881
_diffrn_reflns_av_sigmaI/netI    0.2450
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35892
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.9493
_exptl_absorpt_correction_T_min  0.9396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.2205
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                2673
_reflns_number_total             6797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210542r_si_002_2.cif
_cod_data_source_block           apx914_full
_cod_original_cell_volume        3690(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117730