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_7046206
_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         'C76 H72 Fe2 N4 Na2 O2 P2, 2(C6 H14)'
_chemical_formula_sum            'C88 H100 Fe2 N4 Na2 O2 P2'
_chemical_formula_weight         1465.33
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2018-01-19
_audit_creation_method
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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                 98.746(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8101(5)
_cell_length_b                   15.5735(4)
_cell_length_c                   18.4473(5)
_cell_measurement_reflns_used    6226
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      26.6320
_cell_measurement_theta_min      3.1380
_cell_volume                     3921.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
  1 omega  -33.00   -7.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802   38.0000  -60.0000 26

  2 omega   27.00   85.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  -30.0000 58

  3 omega  -54.00   67.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490    0.0000    0.0000 121

  4 omega   70.00   95.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  179.0000  150.0000 25

  5 omega  -50.00  -25.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -57.0000 -180.0000 25

  6 omega   -3.00   87.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  150.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0395229000
_diffrn_orient_matrix_UB_12      0.0213846000
_diffrn_orient_matrix_UB_13      -0.0216671000
_diffrn_orient_matrix_UB_21      0.0335978000
_diffrn_orient_matrix_UB_22      0.0276026000
_diffrn_orient_matrix_UB_23      -0.0140670000
_diffrn_orient_matrix_UB_31      0.0026681000
_diffrn_orient_matrix_UB_32      -0.0292506000
_diffrn_orient_matrix_UB_33      -0.0290998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27102
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.182
_diffrn_reflns_theta_min         2.814
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         9267
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1018P)^2^+5.6061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5877
_reflns_number_total             9267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01019f2.cif
_cod_data_source_block           Compound6_OPPh3
_cod_depositor_comments
'Adding full bibliography for 7046201--7046206.cif.'
_cod_database_code               7046206
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C40H40Fe1N2O2P2Na1
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.895
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Shared sites
{C18, C18A}
3. Restrained distances
 C44-C43
 1.54 with sigma of 0.01
 C18A-C20A
 1.5 with sigma of 0.02
 C19A-C18A
 1.5 with sigma of 0.02
 C41-C42
 1.54 with sigma of 0.01
 C42-C43
 1.54 with sigma of 0.01
 C40-C41
 1.54 with sigma of 0.01
 C20A-C19A
 2.4 with sigma of 0.04
4. Rigid bond restraints
 C44, C43, C42, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C19A) = Uanis(C19)
Uanis(C20) = Uanis(C20A)
Uanis(C18) = Uanis(C18A)
6. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C18A)=Sof(H18A)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18)=Sof(H18)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C18(H18), C18A(H18A)
7.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C41(H41A,H41B), C43(H43A,H43B), C40(H40A,H40B)
7.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C28(H28), C31(H31), C32(H32), C38(H38), C30(H30), C3(H3), C4(H4),
 C23(H23), C6(H6), C12(H12), C9(H9), C7(H7), C35(H35), C36(H36), C5(H5),
 C37(H37), C29(H29), C26(H26), C15(H15), C13(H13), C11(H11), C17(H17), C10(H10),
  C34(H34), C24(H24), C14(H14), C16(H16), C25(H25)
7.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C44(H44A,H44B,
 H44C), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              68493
_olex2_submission_special_instructions 'No special instructions were received'