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_4088557
_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         'C38 H66 Fe N P2, B F4, C H2 Cl2'
_chemical_formula_sum            'C39 H68 B Cl2 F4 Fe N P2'
_chemical_formula_weight         826.44
_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   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                90.00
_cell_angle_beta                 97.456(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5166(12)
_cell_length_b                   12.5602(13)
_cell_length_c                   28.911(3)
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.189
_cell_measurement_theta_min      2.578
_cell_volume                     4146.6(7)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            29901
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.42
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.9132
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7303
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0581P)^2^+5.6101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                5539
_reflns_number_total             7303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00179_si_002.cif
_cod_data_source_block           '[4(NCMe)]PF6'
_cod_original_cell_volume        4146.7(7)
_cod_database_code               4088557
_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
 B1-F1
 1.45 with sigma of 0.01
 F15-F1
 2.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F0AA \\sim F1 \\sim F3 \\sim F4 \\sim F6 \\sim F11 \\sim F15 \\sim B1: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: F0AA(0.5) F1(0.5) F3(0.5) F4(0.5) F6(0.5) F11(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C19(H19), C25(H25), C31(H31)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C39(H39A,H39B)
5.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), C38(H38A,H38B,H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'