Hydride Transfer from Iron(II) Hydride Compounds to NAD(P)+ Analogues
Zhang, Fanjun; Jia, Jiong; Dong, Shuli; Wang, Wenguang; Tung, Chen-Ho; Organometallics 35 (2016) 1151–; doi:10.1021/acs.organomet.6b00179

data_4088563
_publ_section_title
;
 Hydride Transfer from Iron(II) Hydride Compounds to NAD(P)+ Analogues
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1151
_journal_paper_doi               10.1021/acs.organomet.6b00179
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C49 H51 Fe N2 P2, F6 P, 0.5(C5 H12)'
_chemical_formula_sum            'C51.5 H57 F6 Fe N2 P3'
_chemical_formula_weight         966.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                71.781(4)
_cell_angle_beta                 88.828(4)
_cell_angle_gamma                89.767(4)
_cell_formula_units_Z            4
_cell_length_a                   14.719(6)
_cell_length_b                   18.051(7)
_cell_length_c                   19.797(7)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.805
_cell_measurement_theta_min      2.510
_cell_volume                     4995(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58355
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9688
_exptl_absorpt_correction_T_min  0.9473
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.104
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         17559
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+23.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                11477
_reflns_number_total             17559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00179_si_002.cif
_cod_data_source_block           '[CpFe(dppe)1,4-BzPyH]PF6'
_cod_depositor_comments
;

2020-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C103 H114 F12 Fe2 N4 P6'
_cod_original_formula_weight         1933.50
_cod_original_formula_moiety         '2(C49 H51 Fe N2 P2), 2(F6 P), C5 H12'
_cod_original_formula_units_Z            2
_cod_database_code               4088563
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C100-C101
 1.55 with sigma of 0.01
 C101-C102
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C39(H39A,H39B), C43(H43A,H43B), C60(H60A,
 H60B), C61(H61A,H61B), C88(H88A,H88B), C92(H92A,H92B), C100(H10D,H10E),
 C101(H10F,H10G), C102(H10H,H10I)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41),
 C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C63(H63), C64(H64),
  C65(H65), C66(H66), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72),
 C73(H73), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C81(H81), C82(H82),
  C83(H83), C84(H84), C85(H85), C89(H89), C90(H90), C91(H91), C94(H94),
 C95(H95), C96(H96), C97(H97), C98(H98)
4.c 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), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C99(H99A,H99B,H99C), C103(H10J,H10K,
 H10L)
;
_olex2_submission_special_instructions 'No special instructions were received'