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_7046202
_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         'C60 H63 Bi Fe3 N6, 4(C4 H8 O)'
_chemical_formula_sum            'C76 H95 Bi Fe3 N6 O4'
_chemical_formula_weight         1533.10
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-01-23
_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                93.978(2)
_cell_angle_beta                 107.059(2)
_cell_angle_gamma                105.219(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4649(19)
_cell_length_b                   14.607(2)
_cell_length_c                   18.529(3)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.33
_cell_measurement_theta_min      2.31
_cell_volume                     3319.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31442
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.810
_diffrn_reflns_theta_min         1.689
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.341
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0570 before and 0.0415 after correction. The Ratio of minimum to maximum transmission is 0.8437. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.346
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         14110
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12654
_reflns_number_total             14110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01019f2.cif
_cod_data_source_block           Compound8
_cod_depositor_comments
'Adding full bibliography for 7046201--7046206.cif.'
_cod_database_code               7046202
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C76
 1.4 with sigma of 0.02
 C69-C70
 1.5 with sigma of 0.005
 C70-C71
 1.5 with sigma of 0.005
 C71-C72
 1.5 with sigma of 0.005
 C74-C75
 1.5 with sigma of 0.01
 C73-O4
 1.4 with sigma of 0.02
 C76-C75
 1.5 with sigma of 0.02
 C73-C75
 3.1 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O4) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Rigid body (RIGU) restrains
 C76, C75, C74, C73, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C48(H48), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C64(H64A,H64B), C69(H69A,H69B), C67(H67A,H67B), C72(H72A,
 H72B), C68(H68A,H68B), C63(H63A,H63B), C61(H61A,H61B), C62(H62A,H62B),
 C66(H66A,H66B), C70(H70A,H70B), C71(H71A,H71B), C76(H76A,H76B), C74(H74A,H74B),
  C75(H75A,H75B), C73(H73A,H73B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C32(H32), C53(H53), C18(H18), C39(H39), C4(H4), C52(H52),
 C46(H46), C59(H59), C60(H60), C5(H5), C26(H26), C33(H33), C35(H35), C6(H6),
 C55(H55), C15(H15), C7(H7), C45(H45), C58(H58), C40(H40), C34(H34), C56(H56),
 C12(H12), C27(H27), C3(H3), C47(H47), C54(H54), C13(H13), C17(H17), C44(H44),
 C14(H14), C19(H19), C57(H57), C43(H43), C36(H36), C16(H16), C37(H37), C38(H38),
  C20(H20)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C49(H49A,H49B,H49C), C29(H29A,H29B,H29C), C10(H10A,H10B,
 H10C), C50(H50A,H50B,H50C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              20780
_olex2_submission_special_instructions 'No special instructions were received'