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_1559910
_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 H31 B Fe N P'
_chemical_formula_sum            'C28 H31 B Fe N P'
_chemical_formula_weight         479.17
_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             2020-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   15.3228(2)
_cell_length_b                   26.7339(3)
_cell_length_c                   35.8973(4)
_cell_measurement_temperature    293(2)
_cell_volume                     14484.6(3)
_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_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            77393
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         2.928
_exptl_absorpt_coefficient_mu    5.738
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             6048
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1807
_refine_ls_number_reflns         25279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15495
_reflns_number_total             25279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06787c2.cif
_cod_data_source_block           complex-3
_cod_depositor_comments
;
Adding full bibliography for 1559907--1559911.cif.

2022-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C168 H186 B6 Fe6 N6 P6'
_cod_original_formula_weight         2875.00
_cod_original_formula_moiety         '6(C28 H31 B Fe N P)'
_cod_original_formula_units_Z            4
_cod_database_code               1559910
_shelxl_version_number           2013-4
_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:
 C19(H19), C20(H20), C7AA(H7AA), C99(H99), C17(H17), C7BA(H7BA), C120(H120),
 C42(H42), C67(H67), C108(H108), C24(H24), C105(H105), C4AA(H4AA), C57(H57),
 C46(H46), C92(H92), C126(H126), C109(H109), C3BA(H3BA), C129(H129), C27(H27),
 C54(H54), C130(H130), C114(H114), C29(H29), C22(H22), C95(H95), C26(H26),
 C101(H101), C28(H28), C117(H117), C1AA(H1AA), C103(H103), C9AA(H9AA), C36(H36),
  C40(H40), C122(H122), C123(H123), C16(H16), C45(H45), C38(H38), C63(H63),
 C106(H106), C32(H32), C124(H124), C1BA(H1BA), C127(H127), C115(H115), C59(H59),
  C51(H51), C13(H13), C31(H31), C52(H52), C102(H102), C3AA(H3AA), C43(H43),
 C100(H100), C116(H116), C6BA(H6BA), C2AA(H2AA), C61(H61), C121(H121), C14(H14),
  C66(H66), C25(H25), C53(H53), C30(H30), C94(H94), C15(H15), C60(H60),
 C58(H58), C93(H93), C0BA(H0BA), C8AA(H8AA), C37(H37), C39(H39), C4BA(H4BA),
 C5BA(H5BA), C64(H64), C65(H65), C44(H44), C107(H107), C21(H21), C128(H128)
2.b Idealised Me refined as rotating group:
 C192(H19A,H19B,H19C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C182(H18G,H18H,H18I),
 C189(H18A,H18B,H18C), C6(H6A,H6B,H6C), C152(H15A,H15B,H15C), C148(H14A,H14B,
 H14C), C191(H19D,H19E,H19F), C190(H19G,H19H,H19I), C172(H17A,H17B,H17C),
 C10(H10A,H10B,H10C), C158(H15J,H15K,H15L), C179(H17J,H17K,H17L), C171(H17D,
 H17E,H17F), C169(H16J,H16K,H16L), C181(H18J,H18K,H18L), C170(H17G,H17H,H17I),
 C7(H7A,H7B,H7C), C188(H18D,H18E,H18F), C180(H18M,H18N,H18O), C162(H16A,H16B,
 H16C), C150(H15D,H15E,H15F), C151(H15G,H15H,H15I), C178(H17M,H17N,H17O),
 C160(H16D,H16E,H16F), C159(H15M,H15N,H15O), C149(H14D,H14E,H14F), C168(H16M,
 H16N,H16O), C161(H16G,H16H,H16I)
;
_shelx_res_checksum              62559
_olex2_submission_special_instructions 'No special instructions were received'