Aminotroponiminates: ligand-centred, reversible redox events under oxidative conditions in sodium and bismuth complexes.
Hanft, Anna; Lichtenberg, Crispin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10578–10589; doi:10.1039/c8dt01019f

data_7046203
_publ_section_title
;
 Aminotroponiminates: ligand-centred, reversible redox events under
 oxidative conditions in sodium and bismuth complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10578
_journal_page_last               10589
_journal_paper_doi               10.1039/c8dt01019f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H22 Fe N2'
_chemical_formula_sum            'C20 H22 Fe N2'
_chemical_formula_weight         346.24
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-23 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.5012(14)
_cell_length_b                   5.7094(3)
_cell_length_c                   10.1021(5)
_cell_measurement_reflns_used    4543
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.47
_cell_volume                     1643.86(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12552
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.756
_diffrn_reflns_theta_min         1.429
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1391 before and 0.0816 after correction. The Ratio of minimum to maximum transmission is 0.9127. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0970
_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^)+(0.0320P)^2^+25.9250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2314
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                3323
_reflns_number_total             4047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01019f2.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
'Adding full bibliography for 7046201--7046206.cif.'
_cod_database_code               7046203
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.87(8)
 0.13(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) = Uanis(C2)
Uanis(C12) = Uanis(C16A) = Uanis(C16)
Uanis(C8) = Uanis(C17A) = Uanis(C17)
Uanis(C13A) = Uanis(C13) = Uanis(C9)
Uanis(C14A) = Uanis(C14) = Uanis(C10)
Uanis(C15) = Uanis(C15A) = Uanis(C11)
4. Rigid body (RIGU) restrains
 C1, C2, C7, C6, C5, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C8, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C13A)=
 Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(C16)=Sof(H16)=Sof(C14)=Sof(H14)=Sof(C13)=Sof(H13)=Sof(C17)=Sof(H17)=
 Sof(C15)=Sof(H15)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C13A(H13A), C14A(H14A)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C7(H7), C10(H10), C16(H16), N2(H2), C14(H14), C13(H13),
 C17(H17), C6(H6), C3(H3), C4(H4), C5(H5), C9(H9), C15A(H15A), C16A(H16A),
 C17A(H17A)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              63255
_olex2_submission_special_instructions 'No special instructions were received'