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_1559911
_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 H33 B Fe N P'
_chemical_formula_sum            'C28 H33 B Fe N P'
_chemical_formula_weight         481.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-09-22 deposited with the CCDC.	2021-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.119(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.668(4)
_cell_length_b                   10.792(4)
_cell_length_c                   21.922(8)
_cell_measurement_reflns_used    6107
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.206
_cell_measurement_theta_min      2.686
_cell_volume                     2522.1(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9894
_diffrn_measured_fraction_theta_max 0.9894
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18179
_diffrn_reflns_theta_full        27.5946
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1122 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.7977.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.2672
_exptl_crystal_description       block
_exptl_crystal_F_000             1018.1112
_refine_diff_density_max         0.4432
_refine_diff_density_min         -0.4148
_refine_diff_density_rms         0.0730
_refine_ls_d_res_high            0.7664
_refine_ls_d_res_low             7.5843
_refine_ls_goodness_of_fit_ref   1.0753
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0753
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -11
_reflns_number_gt                4527
_reflns_number_total             5800
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06787c2.cif
_cod_data_source_block           complex-2
_cod_depositor_comments
;
Adding full bibliography for 1559907--1559911.cif.

2022-09-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C112 H132 B4 Fe4 N4 P4'
_cod_original_formula_weight         1924.90
_cod_original_formula_moiety         '4(C28 H33 B Fe N P)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2522.1(15)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1559911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C12(H12), C18(H18), C4(H4), C5(H5), C17(H17), C16(H16),
 C8(H8), C3(H3), C15(H15), C11(H11), C10(H10), C9(H9)
2.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C28(H28a,H28b,
 H28c), C26(H26a,H26b,H26c)
;
_olex2_submission_special_instructions 'No special instructions were received'