Reactivity of (Pyridine-Diimine)Fe Alkyl Complexes with Carbon Dioxide
Lau, Ka-Cheong; Jordan, Richard F.; Organometallics 35 (2016) 3658–; doi:10.1021/acs.organomet.6b00470

data_4088812
_publ_section_title
;
 Reactivity of (Pyridine-Diimine)Fe Alkyl Complexes with Carbon Dioxide
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3658
_journal_paper_doi               10.1021/acs.organomet.6b00470
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C37 H55 Fe N3 P'
_chemical_formula_sum            'C37 H55 Fe N3 P'
_chemical_formula_weight         628.66
_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             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.567(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2088(12)
_cell_length_b                   12.6102(8)
_cell_length_c                   16.3707(11)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.25
_cell_measurement_theta_min      25.02
_cell_volume                     3492.3(4)
_computing_cell_refinement       'SAINT V.8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v.2014.9-0 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V.8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30607
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1604 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.8277.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     2190
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0751
_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^)+(0.0257P)^2^+14.8502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5039
_reflns_number_total             6181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00470_si_002.cif
_cod_data_source_block           (PDI)Fe(Me)PMe3
_cod_database_code               4088812
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.793
_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. Restrained distances
 C36A-C35A \\sim C36-C35 \\sim C37A-C35A \\sim C37-C35 \\sim C28A-C26A \\sim
C28-C26 \\sim C28A-C27A ~
 C28-C27 \\sim C15-C14 \\sim C15A-C14A \\sim C16-C14 \\sim C16A-C14A \\sim
C7-C5 \\sim C7A-C5A \\sim C7-C6
 \\sim C7A-C6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C35) = Uanis(C35A)
Uanis(Fe1) = Uanis(Fe1A)
Uanis(C1) = Uanis(C1A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(C28) = Uanis(C28A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
Uanis(C13) = Uanis(C13A)
Uanis(C12) = Uanis(C12A)
Uanis(C24A) = Uanis(C24)
Uanis(C13) = Uanis(C13A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(P1A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(Fe1A)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7A)=Sof(C8A)=
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=
 Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=1-FVAR(1)
 Sof(P1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(Fe1)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(C19)=
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(C24)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(C30)=
 Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(C34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C28(H28), C35(H35), C7A(H7A), C14A(H14A), C28A(H28A),
 C35A(H35A)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C20(H20), C21(H21), C22(H22), C30(H30), C31(H31),
 C32(H32), C9A(H9A), C10A(H10A), C11A(H11A), C20A(H20A), C21A(H21A), C22A(H22A),
  C30A(H30A), C31A(H31A), C32A(H32A)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C3A(H3AA,H3AB,H3AC), C2A(H2AA,H2AB,
 H2AC), C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,
 H6AB,H6AC), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F),
 C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C36A(H36D,
 H36E,H36F), C37A(H37D,H37E,H37F)
;
_shelx_res_checksum              78352
_shelx_hkl_checksum              26416
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'