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_1559337
_publ_section_title
;
 Aromatic foldamers as scaffolds for metal second coordination sphere
 design
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC05143H
_journal_year                    2020
_chemical_formula_moiety         'C104 H102 Fe2 N19 O23 S2, 3(C H Cl3)'
_chemical_formula_sum            'C107 H105 Cl9 Fe2 N19 O23 S2'
_chemical_formula_weight         2519.96
_chemical_name_systematic        q3pn2afe
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-14
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-14 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.379(9)
_cell_length_b                   22.277(5)
_cell_length_c                   31.801(6)
_cell_measurement_reflns_used    46092
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      47.238
_cell_measurement_theta_min      2.246
_cell_volume                     29704(11)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku MM07'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46092
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        47.238
_diffrn_reflns_theta_max         47.238
_diffrn_reflns_theta_min         2.246
_exptl_absorpt_coefficient_mu    3.826
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       block
_exptl_crystal_F_000             10408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1474
_refine_ls_number_reflns         13285
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1284
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3409
_refine_ls_wR_factor_ref         0.3765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             13285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05143h2.cif
_cod_data_source_block           q3pn2afe_a_sq
_cod_database_code               1559337
_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
 C04O-C041
 1.54 with sigma of 0.02
 C041-C03M
 1.54 with sigma of 0.02
 C04O-C04F
 2.6 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C04O, C04F, C041, C03M, O008
 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:
 C03E(H03H), C03F(H03I), C03Y(H1AA), C040(H040), C041(H041), C048(H048),
 C04A(H04L), C04G(H04Y), C04K(H6AA), C04P(H7AA)
4.b Secondary CH2 refined with riding coordinates:
 C01S(H01B,H01C), C030(H03A,H03B), C036(H03C,H03D), C03C(H03F,H03G), C03J(H03M,
 H03N), C03M(H03P,H03Q), C03U(H03X,H03Y), C03V(H03Z,H), C03W(H03,HA), C042(H04A,
 H04B)
4.c Aromatic/amide H refined with riding coordinates:
 N00R(H00R), N012(H012), N013(H013), N019(H019), N01A(H01A), N01K(H01K),
 C01P(H01P), C020(H020), C027(H027), C02M(H02M), C02N(H02N), C02S(H02S),
 C031(H031), C033(H033), C037(H037), C038(H038), C039(H039), C03B(H03E),
 C03G(H03J), C03H(H03K), C03I(H03L), C03L(H03O), C03O(H03R), C03P(H03S),
 C03Q(H03T), C03R(H03U), C03S(H03V), C03T(H03W), C03X(H0AA), C03Z(H2AA)
4.d Idealised Me refined as rotating group:
 C02X(H02A,H02B,H02C), C044(H04C,H04D,H04E), C045(H04F,H04G,H04H), C047(H04I,
 H04J,H04K), C04B(H04M,H04N,H04O), C04C(H04P,H04Q,H04R), C04D(H04S,H04T,H04U),
 C04F(H04V,H04W,H04X), C04I(H04Z,HB,HC), C04J(H04,HD,HE), C04L(H3AA,HF,HG),
 C04M(H4AA,HH,HI), C04O(H5AA,HJ,HK), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              11381
_shelx_fab_checksum              52764
_olex2_submission_original_sample_id q3pn2afe
_olex2_submission_special_instructions 'No special instructions were received'