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_4089203
_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 Cl Fe N P2'
_chemical_formula_sum            'C38 H44 Cl Fe N P2'
_chemical_formula_weight         667.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-12-07
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.897(7)
_cell_length_b                   17.545(12)
_cell_length_c                   17.653(12)
_cell_measurement_reflns_used    3976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.482
_cell_measurement_theta_min      2.196
_cell_volume                     3375(4)
_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 0.975
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19606
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.194
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.1823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1812 before and 0.0954 after correction.
The Ratio of minimum to maximum transmission is 0.2445.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       stick
_exptl_crystal_F_000             1408
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1609 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4500
_reflns_number_total             5950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00907_si_002.cif
_cod_data_source_block           1Cl
_cod_database_code               4089203
_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:
 C37(H37), C38(H38), C28(H28), C26(H26), C32(H32), C24(H24), C22(H22),
 C34(H34), C20(H20), C36(H36), C16(H16), C29(H29), C23(H23), C35(H35), C25(H25),
  C30(H30), C31(H31), C18(H18), C17(H17), C19(H19)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'