Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by an Amidinato-diolefin Ligand: Characterization and Catalytic Application
Lichtenberg, Crispin; Adelhardt, Mario; Wörle, Michael; Büttner, Torsten; Meyer, Karsten; Grützmacher, Hansjörg; Organometallics 34 (2015) 3079–; doi:10.1021/acs.organomet.5b00395

data_4085917
_publ_section_title
;
 Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by
 an Amidinato-diolefin Ligand: Characterization and Catalytic Application
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3079
_journal_paper_doi               10.1021/acs.organomet.5b00395
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C49 H51 N2 Na O3'
_chemical_formula_sum            'C49 H51 N2 Na O3'
_chemical_formula_weight         738.90
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.145(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.915(5)
_cell_length_b                   8.5483(16)
_cell_length_c                   20.189(4)
_cell_measurement_temperature    101.1
_cell_volume                     3953.9(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.1
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.912
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8862
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.479
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.626829
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0741P)^2^+10.0053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7042
_reflns_number_total             8862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_original_cell_volume        3953.9(13)
_cod_database_code               4085917
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6369(16) 0.3631(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C48) = Uanis(C48A)
Uanis(C47) = Uanis(C47A)
Uanis(C49) = Uanis(C49A)
Uanis(O3A) = Uanis(O3)
4. Others
 Sof(O3)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(H46C)=Sof(H46D)=Sof(C48A)=Sof(H48C)=
 Sof(H48D)=Sof(C47A)=Sof(H47C)=Sof(H47D)=1-FVAR(1)
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(O3A)=Sof(C49)=Sof(H49C)=Sof(H49D)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C49A(H49A,H49B), C41(H41A,H41B), C42(H42A,H42B), C46(H46C,H46D), C46(H46A,
 H46B), C40(H40A,H40B), C38(H38A,H38B), C39(H39A,H39B), C1B(H1BA,H1BB),
 C44(H44A,H44B), C43(H43A,H43B), C47(H47A,H47B), C48(H48A,H48B), C49(H49C,H49D),
  C48A(H48C,H48D), C47A(H47C,H47D)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C30(H30), C11(H11), C4(H4), C5(H5), C8(H8), C12(H12),
 C24(H24), C33(H33), C9(H9), C37(H37), C35(H35), C14(H14), C27(H27), C10(H10),
 C26(H26), C23(H23), C29(H29), C25(H25), C34(H34), C28(H28), C20(H20), C1A(H1A),
  C36(H36)
;
_shelx_res_checksum              86200
_shelx_hkl_checksum              55653
_olex2_submission_special_instructions 'No special instructions were received'