Dehydrogenation of iron amido-borane and resaturation of the imino-borane complex
Zhai, Xiaofang; Pang, Maofu; Feng, Lei; Jia, Jiong; Tung, Chen-Ho; Wang, Wenguang; Chemical Science 12 (2021) 2885–2889; doi:10.1039/D0SC06787C

data_1559908
_publ_section_title
;
 Dehydrogenation of iron amido-borane and resaturation of the imino-borane
 complex
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2885
_journal_page_last               2889
_journal_paper_doi               10.1039/D0SC06787C
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety
'C28 H32 B Fe N P, C32 H12 B F22.5, 2(C4 H8 O), 0.75(F2)'
_chemical_formula_sum            'C68 H60 B2 F24 Fe N O2 P'
_chemical_formula_weight         1487.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-22 deposited with the CCDC.	2021-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                103.817(2)
_cell_angle_beta                 92.601(2)
_cell_angle_gamma                92.604(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9415(3)
_cell_length_b                   14.6375(4)
_cell_length_c                   19.3031(5)
_cell_measurement_reflns_used    14563
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.0670
_cell_volume                     3541.17(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -99.00 -39.00   1.00    0.35    --  -48.45 137.00-122.00   60
  2  \w   -110.00 -67.00   1.00    0.35    --  -48.45-133.00  -8.00   43
  3  \w   -102.00 -64.00   1.00    0.35    --  -48.45-137.00 174.00   38
  4  \w     38.00  69.00   1.00    0.35    --   48.45-133.00  -8.00   31
  5  \w     56.00  83.00   1.00    0.35    --   48.45-137.00 174.00   27
  6  \w    -61.00 -35.00   1.00    3.00    --  -86.25 137.00-122.00   26
  7  \w   -100.00 -74.00   1.00    3.00    --  -86.25 137.00-122.00   26
  8  \w    -97.00 -56.00   1.00    3.00    --  -86.25 133.00  60.00   41
  9  \w    141.00 167.00   1.00    3.00    --  106.49 137.00-122.00   26
 10  \w     85.00 139.00   1.00    3.00    --  106.49 137.00-122.00   54
 11  \w     97.00 122.00   1.00    3.00    --  106.49-133.00  -8.00   25
 12  \w     95.00 126.00   1.00    3.00    --  106.49-137.00 174.00   31
 13  \w     38.00  94.00   1.00    3.00    --  106.49-137.00 174.00   56
 14  \w     91.00 167.00   1.00    3.00    --  106.49 133.00  60.00   76
 15  \w   -120.00 -26.00   1.00    0.35    --  -48.45 -77.00 150.00   94
 16  \w    -96.00 -40.00   1.00    0.35    --  -48.45 133.00  60.00   56
 17  \w     26.00 121.00   1.00    0.35    --   48.45  77.00  60.00   95
 18  \w    -99.00 -63.00   1.00    3.00    --  -86.25-137.00 174.00   36
 19  \w   -125.00-100.00   1.00    3.00    --  -86.25-133.00  -8.00   25
 20  \w   -157.00 -73.00   1.00    3.00    --  -86.25 -38.00  30.00   84
 21  \w     34.00 121.00   1.00    3.00    --  106.49 -57.00 -60.00   87
 22  \w     36.00 120.00   1.00    3.00    --  106.49 -38.00 -60.00   84
 23  \w     74.00 120.00   1.00    3.00    --  106.49 -38.00 120.00   46
 24  \w     76.00 121.00   1.00    3.00    --  106.49 -57.00 150.00   45
 25  \w     38.00  73.00   1.00    3.00    --  106.49 -57.00 150.00   35
 26  \w     34.00  60.00   1.00    3.00    --  106.49 -38.00 120.00   26
 27  \w    131.00 178.00   1.00    3.00    --  106.49  19.00-120.00   47
 28  \w     32.00 116.00   1.00    3.00    --  106.49 -19.00-150.00   84
 29  \w     96.00 177.00   1.00    3.00    --  106.49 125.00 -60.00   81
 30  \w     95.00 123.00   1.00    3.00    --  106.49  19.00-120.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081146000
_diffrn_orient_matrix_UB_12      -0.0229691000
_diffrn_orient_matrix_UB_13      0.0738253000
_diffrn_orient_matrix_UB_21      -0.0050827000
_diffrn_orient_matrix_UB_22      0.1053841000
_diffrn_orient_matrix_UB_23      0.0364090000
_diffrn_orient_matrix_UB_31      -0.1189792000
_diffrn_orient_matrix_UB_32      -0.0123857000
_diffrn_orient_matrix_UB_33      -0.0013078000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35930
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic intense blue'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         12459
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1493P)^2^+3.1167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10145
_reflns_number_total             12459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06787c2.cif
_cod_data_source_block           complex-3H
_cod_depositor_comments
'Adding full bibliography for 1559907--1559911.cif.'
_cod_database_code               1559908
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FePNBF
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C65, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F58, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1, F57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
F1 \\sim C65: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(F1) \\sim Ueq, Uanis(F58) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F1) \\sim Ueq, Uanis(F57) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.05
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F58(0.5) F57(0.5) H2AA(0.5) H2AB(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) F2(0.5) F1(0.5)
 F0AA(0.5) F2AA(0.5) F1AA(0.5) F3(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C45(H45), C3AA(H3AA), C47(H47), C7AA(H7AA), C43(H43), C37(H37),
 C41(H41), C39(H39), C34(H34), C32(H32), C18(H18), C13(H13), C6AA(H6AA),
 C22(H22), C24(H24), C15(H15), C14(H14), C28(H28), C16(H16), C30(H30), C20(H20),
  C26(H26), C19(H19), C21(H21), C25(H25), C27(H27), C83(H83), C97(H97),
 C99(H99), C2AA(H2AA), C2AA(H2AB)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C100(H10D,H10E,H10F), C82(H82A,H82B,H82C), C96(H96A,H96B,H96C),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              56654
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.302
_oxdiff_exptl_absorpt_empirical_full_min 0.520