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_1559907
_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         'C12 H22 B Fe N'
_chemical_formula_sum            'C12 H22 B Fe N'
_chemical_formula_weight         246.96
_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                 98.207(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5601(3)
_cell_length_b                   7.39591(20)
_cell_length_c                   14.8102(4)
_cell_measurement_reflns_used    3932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.4680
_cell_measurement_theta_min      3.4920
_cell_volume                     1361.68(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.989
_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    -78.00 -52.00   1.00    0.10    --  -48.45  98.00  74.00   26
  2  \w     49.00  80.00   1.00    0.10    --   48.45 -98.00 -32.00   31
  3  \w   -159.00-103.00   1.00    0.70    --  -86.25 -98.00 -32.00   56
  4  \w    -73.00 -48.00   1.00    0.70    --  -86.25  98.00  74.00   25
  5  \w    105.00 161.00   1.00    0.70    --  107.75  98.00  74.00   56
  6  \w     56.00  82.00   1.00    0.70    --  107.75 -98.00 -32.00   26
  7  \w    -42.00   6.00   1.00    0.10    --  -48.45  98.00  74.00   48
  8  \w    -56.00  25.00   1.00    0.10    --  -48.45  37.00 -30.00   81
  9  \w   -116.00 -73.00   1.00    0.10    --  -48.45-125.00 120.00   43
 10  \w   -156.00 -89.00   1.00    0.70    --  -86.25 -99.00  30.00   67
 11  \w     68.00 119.00   1.00    0.70    --  107.75 -19.00 -90.00   51
 12  \w     39.00 126.00   1.00    0.70    --  107.75 -77.00 -30.00   87
 13  \w     35.00 109.00   1.00    0.70    --  107.75 -99.00-180.00   74
 14  \w     81.00 106.00   1.00    0.70    --  107.75 -37.00  90.00   25
 15  \w     32.00  63.00   1.00    0.70    --  107.75 -19.00 -90.00   31
 16  \w     38.00  76.00   1.00    0.70    --  107.75 -37.00  90.00   38
;
_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      -0.0032868000
_diffrn_orient_matrix_UB_12      -0.1841515000
_diffrn_orient_matrix_UB_13      0.0481359000
_diffrn_orient_matrix_UB_21      0.0910784000
_diffrn_orient_matrix_UB_22      -0.0693979000
_diffrn_orient_matrix_UB_23      -0.0504721000
_diffrn_orient_matrix_UB_31      0.0841366000
_diffrn_orient_matrix_UB_32      0.0680859000
_diffrn_orient_matrix_UB_33      0.0785181000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6944
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2400
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0437P)^2^+2.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2014
_reflns_number_total             2400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06787c2.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
'Adding full bibliography for 1559907--1559911.cif.'
_cod_database_code               1559907
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeCNB
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C5 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C4AA \\sim C23 \\sim C1AA \\sim
C32 \\sim C3AA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C6 \\sim C28 \\sim C7 \\sim C2AA \\sim C8 \\sim C35: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C9 \\sim C0AA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C13 \\sim C10: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
3. Others
 Sof(C2)=Sof(C1)=Sof(C5)=Sof(C4)=Sof(C3)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=1-FVAR(1)
 Sof(C4AA)=Sof(C3AA)=Sof(C23)=Sof(C1AA)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=
 Sof(H0AC)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C32)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=FVAR(1)
4.a Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C0AA(H0AA,H0AB,H0AC), C2AA(H2AA,H2AB,H2AC), C13(H13A,
 H13B,H13C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C7(H7A,H7B,H7C), C6(H6A,
 H6B,H6C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              95494
_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 2.133
_oxdiff_exptl_absorpt_empirical_full_min 0.706