Solvent Effects on Hydride Transfer from Cp*(P-P)FeH to BNA+ Cation
Zhang, Fanjun; Xu, Xin; Zhao, Yingjie; Jia, Jiong; Tung, Chen-Ho; Wang, Wenguang; Organometallics 36 (2017) 1238–; doi:10.1021/acs.organomet.6b00907

data_4089202
_publ_section_title
;
 Solvent Effects on Hydride Transfer from Cp*(P-P)FeH to BNA+ Cation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1238
_journal_paper_doi               10.1021/acs.organomet.6b00907
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C38 H44 Fe N3 P2, C24 H20 B'
_chemical_formula_sum            'C62 H64 B Fe N3 P2'
_chemical_formula_weight         979.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.450(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.941(3)
_cell_length_b                   32.962(8)
_cell_length_c                   14.906(4)
_cell_measurement_reflns_used    5204
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.277
_cell_measurement_theta_min      2.471
_cell_volume                     6235(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2850
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_number            18969
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.469
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1087 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.8663.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_platon_squeeze_details
;
;
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 2167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.023(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         18969
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0867P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    0.763
_reflns_Friedel_fraction_max     0.781
_reflns_number_gt                7756
_reflns_number_total             18969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00907_si_002.cif
_cod_data_source_block           (1N2)BPh4
_cod_depositor_comments
;

2020-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C124 H128 B2 Fe2 N6 P4'
_cod_original_formula_weight         1959.52
_cod_original_formula_moiety         '2(C38 H44 Fe N3 P2), 2(C24 H20 B)'
_cod_original_formula_units_Z            2
_cod_database_code               4089202
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C115 \\sim C116 \\sim C117 \\sim C118 \\sim C113 \\sim C114: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C77 \\sim C82 \\sim C81 \\sim C80 \\sim C79 \\sim C78: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88),
  C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61),
 C62(H62), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C114(H114),
 C115(H115), C116(H116), C117(H117), C118(H118), C120(H120), C121(H121),
 C122(H122), C123(H123), C124(H124)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C)
;
_olex2_submission_special_instructions 'No special instructions were received'