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_1559909
_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         'C46 H45.4 B Fe N P2, C32 H12 B F24'
_chemical_formula_sum            'C81 H67 B2 F24 Fe N P2'
_chemical_formula_weight         1649.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 93.6090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1206(2)
_cell_length_b                   16.6063(2)
_cell_length_c                   36.1078(5)
_cell_measurement_reflns_used    16148
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.4700
_cell_measurement_theta_min      3.3390
_cell_volume                     7851.73(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.938
_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     26.00 121.00   1.00    0.60    --   48.45  77.00 -60.00   95
  2  \w    100.00 134.00   1.00    5.70    --  106.49 119.00 -26.00   34
  3  \w     93.00 118.00   1.00    5.70    --  106.49 157.00 128.00   25
  4  \w    146.00 173.00   1.00    5.70    --  106.49  19.00  90.00   27
  5  \w     94.00 142.00   1.00    5.70    --  106.49  19.00  90.00   48
  6  \w     34.00  89.00   1.00    0.60    --   48.45-119.00-112.00   55
  7  \w     34.00 109.00   1.00    5.70    --  106.49-119.00-112.00   75
  8  \w     34.00  65.00   1.00    5.70    --  106.49 -57.00 -90.00   31
  9  \w     36.00 104.00   1.00    5.70    --  106.49 -99.00 -90.00   68
 10  \w     34.00 105.00   1.00    5.70    --  106.49 -99.00  60.00   71
 11  \w     80.00 130.00   1.00    5.70    --  106.49-157.00  92.00   50
 12  \w     60.00  85.00   1.00    0.60    --   48.45-157.00  92.00   25
 13  \w     34.00  66.00   1.00    5.70    --  106.49 -57.00 120.00   32
 14  \w     34.00  66.00   1.00    5.70    --  106.49 -57.00  60.00   32
 15  \w    -70.00 -25.00   1.00    0.60    --  -48.45 119.00 -26.00   45
 16  \w    -73.00 -48.00   1.00    5.70    --  -86.25 119.00 -26.00   25
 17  \w    -43.00 -13.00   1.00    5.70    --  -86.25  38.00  90.00   30
 18  \w    -43.00 -13.00   1.00    5.70    --  -86.25  38.00 150.00   30
 19  \w    -93.00 -68.00   1.00    0.60    --  -48.45 157.00 128.00   25
 20  \w    -92.00 -67.00   1.00    5.70    --  -86.25 157.00 128.00   25
 21  \w    -66.00 -14.00   1.00    5.70    --  -86.25  57.00-180.00   52
 22  \w   -119.00 -78.00   1.00    5.70    --  -86.25-119.00-112.00   41
 23  \w   -110.00 -85.00   1.00    0.60    --  -48.45-157.00  92.00   25
 24  \w   -120.00 -73.00   1.00    0.60    --  -48.45-125.00  90.00   47
;
_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      0.0388932000
_diffrn_orient_matrix_UB_12      -0.0323933000
_diffrn_orient_matrix_UB_13      0.0383244000
_diffrn_orient_matrix_UB_21      0.0294410000
_diffrn_orient_matrix_UB_22      0.0861471000
_diffrn_orient_matrix_UB_23      0.0124040000
_diffrn_orient_matrix_UB_31      -0.1069649000
_diffrn_orient_matrix_UB_32      0.0118688000
_diffrn_orient_matrix_UB_33      0.0143743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53180
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.333
_diffrn_reflns_theta_min         4.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic intense brown'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         15452
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1302P)^2^+9.8748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12155
_reflns_number_total             15452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06787c2.cif
_cod_data_source_block           complex-3H-PPh3
_cod_depositor_comments
'Adding full bibliography for 1559907--1559911.cif.'
_cod_database_code               1559909
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FePNCBF
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.766
_diffrn_oxdiff_digest_frames
;
0108b80f52e7e11a7e2edee74daa99f60901013f45e
;
_diffrn_oxdiff_digest_hkl
;
01dbe3db38daa4435f3082fd178c10ef8498db
;
_reflns_odcompleteness_completeness 98.52
_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. Uiso/Uaniso restraints and constraints
F7 \\sim F3AA \\sim F01X \\sim F2AA \\sim F02G \\sim F13: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
F0AA \\sim F01V \\sim F5 \\sim F02I \\sim F4 \\sim F00L: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C1AA \\sim C10 \\sim C0AA \\sim C9 \\sim C3AA \\sim C2AA \\sim C8 \\sim C7
\\sim C4AA \\sim C6: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(F1AA) \\sim Ueq, Uanis(F015) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F019)
\\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F01Y) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: F00L(0.6) F015(0.7) F019(0.7) F01V(0.6) F01X(0.5) F01Y(0.7)
 F02G(0.5) F02I(0.6) C6(0.6) H6A(0.6) H6B(0.6) H6C(0.6) C10(0.6) H10A(0.6)
 H10B(0.6) H10C(0.6) C7(0.6) H7A(0.6) H7B(0.6) H7C(0.6) C9(0.6) H9A(0.6)
 H9B(0.6) H9C(0.6) C8(0.6) H8A(0.6) H8B(0.6) H8C(0.6) F7(0.5) C0AA(0.4)
 H0AA(0.4) H0AB(0.4) H0AC(0.4) C1AA(0.4) H1AA(0.4) H1AB(0.4) C2AA(0.4)
 H2AA(0.4) H2AB(0.4) C3AA(0.4) H3AA(0.4) H3AB(0.4) C4AA(0.4) H4AA(0.4)
 H4AB(0.4) F4(0.4) F5(0.4) F0AA(0.4) F2(0.3) F1AA(0.3) F10(0.3) F2AA(0.5)
 F3AA(0.5) F13(0.5)
4.a Ternary CH refined with riding coordinates:
 N1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C4AA(H4AA,H4AB)
4.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00C(H00C), C00I(H00I), C00M(H00M), C00N(H00N),
 C00Q(H00Q), C16(H16), C00W(H00W), C14(H14), C012(H012), C014(H014), C15(H15),
 C13(H13), C01C(H01C), C30(H30), C01O(H01O), C42(H42), C46(H46), C36(H36),
 C31(H31), C34(H34), C33(H33), C28(H28), C27(H27), C32(H32), C43(H43), C22(H22),
  C40(H40), C44(H44), C45(H45), C26(H26), C21(H21), C18(H18), C20(H20),
 C19(H19), C24(H24), C37(H37), C39(H39), C38(H38), C25(H25)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C8(H8A,H8B,H8C), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              78814
_shelx_fab_checksum              71111
_platon_squeeze_void_probe_radius 1.20
_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 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.686