Foldamer-based helicate displaying reversible switching between two distinct conformers.
Jeon, Hae-Geun; Lee, Hyun Kyung; Lee, Seungwon; Jeong, Kyu-Sung; Chemical communications (Cambridge, England) 54 (2018) 5740–5743; doi:10.1039/c8cc02758g

data_7121706
_publ_section_title
;
 Foldamer-based helicate displaying reversible switching between two
 distinct conformers.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5740
_journal_page_last               5743
_journal_paper_doi               10.1039/c8cc02758g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C148 H136 Cl4 N12 O2 Pd2'
_chemical_formula_sum            'C148 H136 Cl4 N12 O2 Pd2'
_chemical_formula_weight         2469.28
_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             2017-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                73.077(2)
_cell_angle_beta                 84.189(3)
_cell_angle_gamma                81.240(4)
_cell_formula_units_Z            4
_cell_length_a                   16.792(2)
_cell_length_b                   23.687(2)
_cell_length_c                   39.551(3)
_cell_measurement_reflns_used    337284
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      50.00
_cell_volume                     14848(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.1322
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            82338
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.499
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.384
_diffrn_source                   'Fixed gap multiple wiggler beamline'
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00162(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3181
_refine_ls_number_reflns         42189
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0925
_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^)+(0.1449P)^2^+27.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25624
_reflns_number_total             42189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02758g2.cif
_cod_data_source_block           IP_Synsyn_complex
_cod_depositor_comments
'Adding full bibliography for 7121704--7121706.cif.'
_cod_database_code               7121706
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O62-C61
 1.4 with sigma of 0.02
 C161-C158
 1.5 with sigma of 0.02
 C460-C158
 1.5 with sigma of 0.02
 C0AA-C158
 1.5 with sigma of 0.02
 C308-C262 \\sim C310-C308 \\sim C311-C308 \\sim C308-C309
 with sigma of 0.01
 C408-C409 \\sim C408-C462 \\sim C411-C408 \\sim C410-C408
 with sigma of 0.01
 C146-C149 \\sim C146-C148 \\sim C146-C147
 with sigma of 0.01
 C142-C145 \\sim C142-C144
 with sigma of 0.02
 C261-C260 \\sim C462-C261 \\sim C462-C463 \\sim C244-C463 \\sim C244-C245
\\sim C260-C245
 with sigma of 0.02
 C462-C461 \\sim C462-C463 \\sim C244-C463 \\sim C244-C245 \\sim C260-C245
\\sim C260-C461
 with sigma of 0.02
3. Restrained planarity
 C244, C245, C260, C261, C262, C263
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
Uanis(C160) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C261) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C1AA) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C460) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C0AA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C155) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C323) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C242) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C317) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C226) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C241) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C67) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C63) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C225) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.01
Uanis(C147) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C154) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C157) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C306) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C307) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C144) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C142) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C145) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C320) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms of 0.03
Uanis(O224) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C237) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
5. Rigid body (RIGU) restrains
 C159, C160, C161, C0AA, C1AA, C460
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.0005
 C261, C262, C263, C308, C309, C310, C311, C408, C409, C410, C411, C461, C462,
 C463
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C408(0.5) C409(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C410(0.5)
 H41A(0.5) H41B(0.5) H41C(0.5) C411(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
 C461(0.5) H461(0.5) C462(0.5) C463(0.5) H463(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C460(0.5)
 H46A(0.5) H46B(0.5) H46C(0.5) C159(0.5) H15S(0.5) H15T(0.5) H15U(0.5)
 C160(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C161(0.5) H16G(0.5) H16H(0.5)
 H16I(0.5) C261(0.5) H261(0.5) C262(0.5) C263(0.5) H263(0.5) C308(0.5)
 C309(0.5) H30G(0.5) H30H(0.5) H30I(0.5) C310(0.5) H31S(0.5) H31T(0.5)
 H31U(0.5) C311(0.5) H31V(0.5) H31W(0.5) H31X(0.5)
7.a Me refined with riding coordinates:
 C237(H23P,H23Q,H23R), C307(H30D,H30E,H30F), C145(H14D,H14E,H14F), C149(H14J,
 H14K,H14L), C460(H46A,H46B,H46C)
7.b Aromatic/amide H refined with riding coordinates:
 N165(H165), N168(H168), N185(H185), N188(H188), N246(H246), N249(H249),
 N266(H266), N269(H269), C7CA(H7CA), C171(H171), C173(H173), C176(H176),
 C177(H177), C180(H180), C182(H182), C191(H191), C193(H193), C197(H197),
 C200(H200), C202(H202), C206(H206), C207(H207), C208(H208), C210(H210),
 C212(H212), C214(H214), C252(H252), C254(H254), C257(H257), C258(H258),
 C272(H272), C274(H274), C277(H277), C278(H278), C281(H281), C283(H283),
 C287(H287), C288(H288), C289(H289), C291(H291), C293(H293), C295(H295),
 C461(H461), C463(H463), N3(H3), N6(H6), N23(H23), N26(H26), N84(H84), N87(H87),
  N104(H104), N107(H107), C9(H9), C11(H11), C14(H14), C15(H15), C18(H18),
 C20(H20), C29(H29), C31(H31), C34(H34), C35(H35), C38(H38), C40(H40), C43(H43),
  C44(H44), C45(H45), C48(H48), C50(H50), C52(H52), C90(H90), C92(H92),
 C95(H95), C96(H96), C99(H99), C101(H101), C110(H110), C112(H112), C115(H115),
 C116(H116), C119(H119), C121(H121), C125(H125), C126(H126), C127(H127),
 C129(H129), C131(H131), C133(H133), C261(H261), C263(H263)
7.c Idealised Me refined as rotating group:
 C225(H22A,H22B,H22C), C226(H22D,H22E,H22F), C228(H22G,H22H,H22I), C229(H22J,
 H22K,H22L), C230(H23A,H23B,H23C), C232(H23D,H23E,H23F), C233(H23G,H23H,H23I),
 C234(H23J,H23K,H23L), C236(H23M,H23N,H23O), C238(H23S,H23T,H23U), C240(H24A,
 H24B,H24C), C241(H24D,H24E,H24F), C242(H24G,H24H,H24I), C243(H24J,H24K,H24L),
 C306(H30A,H30B,H30C), C313(H31A,H31B,H31C), C314(H31D,H31E,H31F), C315(H31G,
 H31H,H31I), C317(H31J,H31K,H31L), C318(H31M,H31N,H31O), C319(H31P,H31Q,H31R),
 C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C323(H32G,H32H,H32I), C324(H32J,
 H32K,H32L), C409(H40A,H40B,H40C), C410(H41A,H41B,H41C), C411(H41D,H41E,H41F),
 C147(H0CA,H0CB,H0CC), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C144(H14A,H14B,H14C), C148(H14G,H14H,H14I),
 C151(H15A,H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,H15H,H15I), C155(H15J,
 H15K,H15L), C156(H15M,H15N,H15O), C157(H15P,H15Q,H15R), C162(H16A,H16B,H16C),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C159(H15S,H15T,H15U), C160(H16D,
 H16E,H16F), C161(H16G,H16H,H16I), C309(H30G,H30H,H30I), C310(H31S,H31T,H31U),
 C311(H31V,H31W,H31X)
7.d Idealised tetrahedral OH refined as rotating group:
 O224(H224), O305(H305), O62(H62), O143(H143)
;
_shelx_res_checksum              56868
_shelx_fab_checksum              28325
_olex2_submission_special_instructions 'No special instructions were received'