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_1559338
_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         'C189 H193 Fe2 N30 O35 S2, C6 H5 Cl'
_chemical_formula_sum            'C195 H198 Cl Fe2 N30 O35 S2'
_chemical_formula_weight         3733.09
_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             2020-09-07
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
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_cell_angle_alpha                97.71(3)
_cell_angle_beta                 104.52(3)
_cell_angle_gamma                97.62(3)
_cell_formula_units_Z            2
_cell_length_a                   17.496(4)
_cell_length_b                   21.656(4)
_cell_length_c                   33.846(7)
_cell_measurement_reflns_used    4007
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      50.8
_cell_measurement_theta_min      9.1
_cell_volume                     12116(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1429
_diffrn_reflns_av_unetI/netI     0.1487
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            78733
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        44.491
_diffrn_reflns_theta_max         44.491
_diffrn_reflns_theta_min         2.290
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_description       prism
_exptl_crystal_F_000             3918
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2417
_refine_ls_number_reflns         18810
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2277
_refine_ls_wR_factor_ref         0.2566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7894
_reflns_number_total             18810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05143h2.cif
_cod_data_source_block           end_a
_cod_database_code               1559338
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C075
 1.54 with sigma of 0.02
 C16-C0AA
 1.54 with sigma of 0.02
 C16-C067
 1.54 with sigma of 0.02
 C081-C18 = O01S-C03M
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C2, C06E, C066, C04J, O00Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C081, C06C, O01S, C03M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C07V, C073, C7, C04P, O009, C02E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C080, C07D, C07B, C05U, O00J, C03R
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C07H, C07Q, C078, C06A, O01Q, C056
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl00, C06P, C06Y, C076, C06Z, C06T, C06S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C075, C16, C0AA, C067, O00X, C048
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C080, C07B, C07D, C05U, O00J, C03R
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C075, C0AA, C16, C067, O00X, C048
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 C4, C081, C18, C06C, O01S, C03M
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 O055, C063
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O06U, C06L, Fe02
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
4.a Ternary CH refined with riding coordinates:
 C051(H051), C052(H052), C05L(H05M), C05P(H05S), C05R(H05V), C060(H060),
 C065(H065), C066(H066), C06I(H06X), C073(H073), C078(H078), C07D(H07M),
 C081(H081), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C03Q(H03A,H03B), C03Z(H03C,H03D), C04J(H04A,H04B), C04M(H04D,H04J), C04P(H04K,
 H04M), C054(H05A,H05B), C057(H05C,H05D), C05A(H05E,H05F), C05D(H05H,H05I),
 C05M(H05N,H05O), C05Q(H05T,H05U), C05U(H05X,H05Y), C05Y(H1AA,HB), C05Z(H2AA,
 HC), C064(H06D,H06E), C067(H06F,H06G), C06A(H06K,H06L), C06C(H06M,H06N)
4.c Aromatic/amide H refined with riding coordinates:
 N00I(H00I), N00M(H00M), N00Q(H00Q), N00R(H00R), N012(H012), N013(H013),
 N01B(H01B), N01F(H01F), N01W(H01W), C021(H021), N023(H023), C029(H029),
 C02H(H02H), C02X(H02X), C030(H030), C033(H033), C036(H036), C039(H039),
 C03S(H03S), C03T(H03T), C03W(H03W), C03X(H03X), C040(H040), C041(H041),
 C043(H043), C045(H045), C047(H047), C04C(H04C), C04E(H04E), C04F(H04F),
 C04G(H04G), C04H(H04H), C04I(H04I), C04L(H04L), C04N(H04N), C04R(H04R),
 C04S(H04S), C04U(H04U), C04V(H04V), C04X(H04X), C050(H050), C053(H053),
 C05C(H05G), C05F(H05J), C05G(H05K), C05H(H05L), C05T(H05W), C05W(H05),
 C05X(H0AA), C061(H061), C06S(H8AA), C06T(H9AA), C06Y(H0BA), C06Z(H1BA),
 C076(H076)
4.d Idealised Me refined as rotating group:
 C05N(H05P,H05Q,H05R), C05V(H05Z,H,HA), C062(H06A,H06B,H06C), C068(H06H,H06I,
 H06J), C06D(H06O,H06P,H06Q), C06E(H06R,H06S,H06T), C06H(H06U,H06V,H06W),
 C06J(H06Y,HD,HE), C06K(H06Z,HF,HG), C06M(H06,HH,HI), C06N(H3AA,HJ,HK),
 C06Q(H4AA,HL,HM), C06R(H5AA,HN,HO), C070(H07A,H07B,H07C), C075(H07D,H07E,H07F),
  C077(H07G,H07H,H07I), C07B(H07J,H07K,H07L), C07F(H07N,H07O,H07P), C07H(H07Q,
 H07R,H07S), C07K(H07T,H07U,H07V), C07L(H07W,H07X,H07Y), C07Q(H07Z,HP,HQ),
 C07T(H07,HR,HS), C07V(H6AA,HT,HU), C07W(H7AA,HV,HW), C080(H08A,H08B,H08C),
 C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C0AA(H0AB,H0AC,H0AD),
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              49560
_shelx_fab_checksum              71306
_olex2_submission_special_instructions 'No special instructions were received'