Dynamic combinatorial libraries of a dimercapto-pillar[5]arene.
Luo, Jinwen; Guo, Yunlong; Li, Ping; Sue, Andrew C.-H.; Cheng, Chuyang; Chemical communications (Cambridge, England) 58 (2022) 8646–8649; doi:10.1039/d2cc02752f

data_7130461
_publ_section_title
;
 Dynamic combinatorial libraries of a dimercapto-pillar[5]arene.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8646
_journal_page_last               8649
_journal_paper_doi               10.1039/d2cc02752f
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety
'C129 H133 O24 S6, 2(C4 H8 O), 3(C3 H6 O), 1.5[tetrahydrofuran], 2[C3H6O], 0.5[Tetrahydrofuran]'
_chemical_formula_sum            'C160 H194 O33 S6'
_chemical_formula_weight         2837.50
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-25 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                98.883(2)
_cell_angle_beta                 93.032(2)
_cell_angle_gamma                103.195(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3614(6)
_cell_length_b                   23.4929(13)
_cell_length_c                   27.5134(14)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      26.261
_cell_measurement_theta_min      2.257
_cell_volume                     7653.4(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72725
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.920
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.9516.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1671
_refine_ls_number_reflns         26604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+5.3946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17028
_reflns_number_total             26604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02752f2.cif
_cod_data_source_block           mo_ccy_ljw_44_6_180k_0m_a
_cod_database_code               7130461
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.964
_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. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00B), C01J(H01B,H01F), C01W(H01G,H01H), C02H(H02A,H02B), C02Y(H02C,
 H02D), C02C(H02E,H02F), C02G(H02G,H02H), C03Y(H03D,H03E), C03K(H03P,H03Q),
 C03R(H03Z,HB), C04N(H11,HG), C04P(H15,HH), C04R(H12,HI), C04V(H13,HN),
 C04Y(H16,HQ), C04F(H17,HV), C026(H02I,H02L), C027(H02M,H02N), C028(H02O,H02Q),
 C034(H4,H24), C037(H5,H25), C042(H04,H26), C045(H18,H31), C046(H14,H32)
3.b Aromatic/amide H refined with riding coordinates:
 C01A(H01A), C01C(H01C), C01D(H01D), C01E(H01E), C01L(H01L), C01N(H01N),
 C01O(H01O), C01S(H01S), C01V(H01V), C02J(H02J), C02K(H02K), C02P(H02P),
 C02R(H02R), C02T(H02T), C02V(H02V), C03D(H03L), C03E(H03M), C03F(H03N),
 C03I(H03O), C03N(H03R), C03T(H03), C03X(H3), C019(H019), C020(H020),
 C024(H024), C025(H025), C029(H029), C038(H038), C039(H039)
3.c Idealised Me refined as rotating group:
 C03W(H03A,H03B,H03C), C03Z(H03F,H03G,H03H), C03C(H03I,H03J,H03K), C03O(H03S,
 H03T,H03U), C03P(H03V,H03W,H03X), C03Q(H03Y,H,HA), C03U(H1,HC,HD), C03V(H2,HE,
 HF), C04J(H04A,H04B,H04C), C04M(H04D,H04E,H04F), C04Q(H04G,H04H,H04I),
 C04S(H22,HJ,HK), C04T(H20,HL,HM), C04U(H04J,H04K,H04L), C04W(H04M,H04N,H04O),
 C04X(H21,HO,HP), C04Z(H19,HR,HS), C04A(H04P,H04Q,H04R), C04B(H04S,H04T,H04U),
 C04C(H04V,H04W,H04X), C04E(H23,HT,HU), C04G(H04Y,HW,HX), C04H(H04Z,HY,HZ),
 C043(H6,H27,H28), C044(H7,H29,H30), C047(H8,H33,H34), C048(H9,H35,H36),
 C049(H10,H37,H38), C050(H05A,H05B,H05C), C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4544
_shelx_hkl_checksum              9178
_shelx_fab_checksum              95378
_olex2_submission_special_instructions 'No special instructions were received'