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_7046204
_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
'C90 H99.5 Fe4 N4 Na4 O9.48, 0.56(C4 H8 O), 0.94(C5 H12), C2 H4 O0.25'
_chemical_formula_sum            'C98.96 H119.35 Fe4 N4 Na4 O10.27'
_chemical_formula_weight         1844.51
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-21
_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                85.773(6)
_cell_angle_beta                 87.331(6)
_cell_angle_gamma                62.126(5)
_cell_formula_units_Z            2
_cell_length_a                   15.062(3)
_cell_length_b                   15.807(3)
_cell_length_c                   21.488(4)
_cell_measurement_reflns_used    9249
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.33
_cell_volume                     4509.7(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0822
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78926
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_min         2.328
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0989 before and 0.0542 after correction. The Ratio of minimum to maximum transmission is 0.9176. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1943
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         15892
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0610P)^2^+8.4760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11097
_reflns_number_total             15892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01019f2.cif
_cod_data_source_block           Compound3_thf1_5
_cod_depositor_comments
'Adding full bibliography for 7046201--7046206.cif.'
_cod_original_cell_volume        4509.9(15)
_cod_database_code               7046204
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C103-C104
 1.54 with sigma of 0.02
 C104-C105
 1.54 with sigma of 0.02
 C100-O12
 1.54 with sigma of 0.02
 O12-C97
 1.54 with sigma of 0.02
 C97-C98
 1.54 with sigma of 0.02
 C98-C99
 1.4 with sigma of 0.02
 C99-C100
 1.4 with sigma of 0.02
 C71A-C70A
 1.54 with sigma of 0.02
 C71A-C72A
 1.54 with sigma of 0.02
 C71-C72
 1.54 with sigma of 0.02
 C70-C71
 1.54 with sigma of 0.02
 C86A-C87A
 1.54 with sigma of 0.02
 C87A-C88A
 1.54 with sigma of 0.02
 C86A-C85A
 1.54 with sigma of 0.02
 C94-C95
 1.54 with sigma of 0.02
 C94-C93
 1.54 with sigma of 0.02
 C95-C96
 1.54 with sigma of 0.02
 H5AA-H95A
 1.115 with sigma of 0.02
 O11-C93
 1.54 with sigma of 0.02
 C96-O11
 1.54 with sigma of 0.02
 C91-C90
 1.54 with sigma of 0.02
 C92-C91
 1.54 with sigma of 0.01
 C4AA-C0AA
 1.54 with sigma of 0.02
 C0AA-C1AA
 1.54 with sigma of 0.02
 C1AA-C2AA
 1.54 with sigma of 0.02
 C2AA-C1AA
 1.54 with sigma of 0.02
 C1AA-C0AA
 1.54 with sigma of 0.02
 C0AA-C4AA
 1.54 with sigma of 0.02
 H2AA-H92A
 1 with sigma of 0.02
 C4AA-C5AA
 1.54 with sigma of 0.02
 O9A-C85A
 1.4 with sigma of 0.02
 C88A-O9A
 1.4 with sigma of 0.02
 C102-C103
 1.54 with sigma of 0.02
 C101-C102
 1.54 with sigma of 0.02
 C96-C94
 2.3 with sigma of 0.01
 C96-C93
 2.3 with sigma of 0.01
 C89-C91
 2.3 with sigma of 0.04
 C2AA-C4AA
 2.5 with sigma of 0.04
 C1AA-C4AA
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C88 \\sim C87 \\sim C86 \\sim C85 \\sim O9 \\sim C85A \\sim O9A \\sim C86A
\\sim C88A \\sim C87A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C71) \\sim Ueq: with sigma of 0.016 and sigma for terminal atoms of 0.032
Uanis(C87) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4AA) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C2AA) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C88) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C85)
\\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C98, C97, O12, C100, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C69, C70A, C72A, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C72, C71, C70, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, C93, C96, C95, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C90, O10, C89, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AA, C0AA, C4AA, C2AA, C5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87A, C88A, C86A, C85A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H37)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=
 Sof(C41A)=Sof(H41A)=1-FVAR(1)
 Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38)=FVAR(1)
 Sof(H69C)=Sof(H69D)=Sof(C70)=Sof(H70C)=Sof(H70D)=Sof(C71)=Sof(H71C)=Sof(H71D)=
 Sof(C72)=Sof(H72C)=Sof(H72D)=1-FVAR(2)
 Sof(H69A)=Sof(H69B)=Sof(C72A)=Sof(H72A)=Sof(H72B)=Sof(C70A)=Sof(H70A)=
 Sof(H70B)=Sof(C71A)=Sof(H71A)=Sof(H71B)=FVAR(2)
 Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(C87A)=
 Sof(H87C)=Sof(H87D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(O9A)=1-FVAR(3)
 Sof(O9)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=
 Sof(H86A)=Sof(H86B)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(3)
 Sof(C105)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C101)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C104)=Sof(H10G)=Sof(H10H)=Sof(C103)=Sof(H10I)=Sof(H10J)=
 Sof(C102)=Sof(H10K)=Sof(H10L)=1-FVAR(4)
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C99)=Sof(H99A)=
 Sof(H99B)=Sof(C100)=Sof(H10M)=Sof(H10N)=Sof(O12)=FVAR(4)
 Fixed Sof: C90(0.5) H90A(0.5) H90B(0.5) C92(0.5) H92A(0.5) H92B(0.5) C89(0.5)
 H89A(0.5) H89B(0.5) C91(0.5) H91A(0.5) H91B(0.5) C96(0.5) H96A(0.5) H96B(0.5)
 O11(0.25) C95(0.5) H95A(0.5) H95B(0.5) C93(0.5) H93A(0.5) H93B(0.5) C94(0.5)
 H94A(0.5) H94B(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C1AA(0.5)
 H1AA(0.5) H1AB(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C4AA(0.5) H4AA(0.5)
 H4AB(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C77(H77A,H77B), C79(H79A,H79B), C78(H78A,H78B), C69(H69A,
 H69B), C69(H69C,H69D), C73(H73A,H73B), C74(H74A,H74B), C76(H76A,H76B),
 C75(H75A,H75B), C72A(H72A,H72B), C70A(H70A,H70B), C87(H87A,H87B), C85(H85A,
 H85B), C98(H98A,H98B), C97(H97A,H97B), C86(H86A,H86B), C99(H99A,H99B),
 C71A(H71A,H71B), C90(H90A,H90B), C92(H92A,H92B), C89(H89A,H89B), C91(H91A,
 H91B), C100(H10M,H10N), C70(H70C,H70D), C71(H71C,H71D), C72(H72C,H72D),
 C88(H88A,H88B), C104(H10G,H10H), C103(H10I,H10J), C102(H10K,H10L), C85A(H85C,
 H85D), C88A(H88C,H88D), C87A(H87C,H87D), C86A(H86C,H86D), C96(H96A,H96B),
 C95(H95A,H95B), C93(H93A,H93B), C94(H94A,H94B), C1AA(H1AA,H1AB), C0AA(H0AA,
 H0AB), C4AA(H4AA,H4AB), C84(H84A,H84B), C83(H83A,H83B), C81(H81A,H81B),
 C82(H82A,H82B)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C45(H45), C29(H29), C51(H51), C46(H46), C44(H44), C12(H12), C7(H7),
 C43(H43), C50(H50), C21(H21), C3(H3), C24(H24), C49(H49), C47(H47), C27(H27),
 C28(H28), C20(H20), C6(H6), C31(H31), C54(H54), C32(H32), C22(H22), C5(H5),
 C60(H60), C4(H4), C48(H48), C37(H37), C63(H63), C23(H23), C30(H30), C34(H34),
 C64(H64), C33(H33), C14(H14), C65(H65), C61(H61), C13(H13), C62(H62), C11(H11),
  C9(H9), C66(H66), C10(H10), C58(H58), C17(H17), C67(H67), C15(H15), C55(H55),
 C16(H16), C68(H68), C38A(H38A), C57(H57), C56(H56), C41(H41), C40(H40),
 C39(H39), C39A(H39A), C40A(H40A), C41A(H41A), C38(H38)
6.c Idealised Me refined as rotating group:
 C105(H10A,H10B,H10C), C101(H10D,H10E,H10F), C2AA(H2AA,H2AB,H2AC), C5AA(H5AA,
 H5AB,H5AC)
;
_shelx_res_checksum              91198
_olex2_submission_special_instructions 'No special instructions were received'