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_7046205
_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         'C40 H42 Bi2 Cl4 Fe2 N4'
_chemical_formula_sum            'C40 H42 Bi2 Cl4 Fe2 N4'
_chemical_formula_weight         1250.23
_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     direct
_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                64.945(2)
_cell_angle_beta                 75.396(2)
_cell_angle_gamma                84.677(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3954(8)
_cell_length_b                   12.5471(8)
_cell_length_c                   14.5794(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    101
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.45
_cell_volume                     1987.5(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      101
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.986
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25022
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.750
_diffrn_reflns_theta_min         2.253
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.847
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0905 before and 0.0503 after correction. The Ratio of minimum to maximum transmission is 0.8154. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8337
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0160P)^2^+24.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6431
_reflns_number_total             8337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01019f2.cif
_cod_data_source_block           Compound7
_cod_depositor_comments
'Adding full bibliography for 7046201--7046206.cif.'
_cod_database_code               7046205
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.335
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C21) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C8) = Uanis(C28)
3. Rigid body (RIGU) restrains
 C21, C27, C26, C25, C24, C23, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C8, N2, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C15, C14, C12, C13, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C20, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C36, C40, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C8(H8), C28(H28)
4.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C23(H23), C27(H27), C3(H3), C6(H6), C17(H17), C20(H20), C4(H4),
 C32(H32), C13(H13), C15(H15), C7(H7), C26(H26), C33(H33), C34(H34), C25(H25),
 C19(H19), C18(H18), C14(H14), C24(H24), C5(H5), C39(H39), C12(H12), C37(H37),
 C36(H36), C16(H16), C38(H38), C40(H40)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C10(H10A,H10B,H10C), C30(H30A,H30B,H30C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              16430
_olex2_submission_special_instructions 'No special instructions were received'