Aromatic foldamers as scaffolds for metal second coordination sphere design
Meunier, Antoine; Singleton, Michael; Kauffmann, Brice; Granier, Thierry; Lautrette, Guillaume; Ferrand, Yann; Huc, Ivan; Chemical Science  (2020) –; doi:10.1039/D0SC05143H

data_1559336
_publ_section_title
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 Aromatic foldamers as scaffolds for metal second coordination sphere
 design
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC05143H
_journal_year                    2020
_chemical_formula_moiety         'C33 H33 Fe2 N3 O12 S2'
_chemical_formula_sum            'C33 H33 Fe2 N3 O12 S2'
_chemical_formula_weight         839.44
_chemical_properties_physical    Air-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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
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_cell_angle_alpha                90.34(3)
_cell_angle_beta                 100.67(3)
_cell_angle_gamma                114.20(3)
_cell_formula_units_Z            2
_cell_length_a                   11.614(2)
_cell_length_b                   11.913(2)
_cell_length_c                   14.995(3)
_cell_measurement_reflns_used    10984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.895
_cell_measurement_theta_min      2.211
_cell_volume                     1851.9(8)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'PILATUS 6M-F'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10984
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        24.895
_diffrn_reflns_theta_max         24.895
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform/Hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0829P)^2^+6.5809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3617
_reflns_number_total             3993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05143h2.cif
_cod_data_source_block           a-fe_fip2011
_cod_database_code               1559336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.879
_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. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C17B)
\\sim Ueq, Uanis(C505) \\sim Ueq, Uanis(C503) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C212)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C211)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20B)=Sof(H20H)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C20A)=Sof(H20D)=Sof(C202)=Sof(H20E)=Sof(H20F)=Sof(H20G)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C39(H39), C20A(H20D), C20B(H20H)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C31(H31A,H31B), C36(H36A,H36B), C17A(H17A,H17B),
 C17B(H17C,H17D)
5.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C34(H34A,H34B,
 H34C), C201(H20A,H20B,H20C), C202(H20E,H20F,H20G), C212(H21A,H21B,H21C),
 C211(H21D,H21E,H21F)
5.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C41(H41)
;
_shelx_res_checksum              28635
_olex2_submission_special_instructions 'No special instructions were received'