Strapped calix[4]pyrrole as a lithium salts selective receptor through separated ion-pair binding.
Hong, Kyeong-Im; Kim, Hyeongcheol; Kim, Younghun; Choi, Moon-Gun; Jang, Woo-Dong; Chemical communications (Cambridge, England) 56 (2020) 10541–10544; doi:10.1039/d0cc04809g

data_7126981
_publ_section_title
;
 Strapped calix[4]pyrrole as a lithium salts selective receptor through
 separated ion-pair binding.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10541
_journal_page_last               10544
_journal_paper_doi               10.1039/d0cc04809g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'Cl, C40 H58 Li N10 O7, 1.5(C2 H3 N)'
_chemical_formula_sum            'C43 H62.5 Cl Li N11.5 O7'
_chemical_formula_weight         894.93
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-03-16 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                88.50(3)
_cell_angle_beta                 86.85(3)
_cell_angle_gamma                77.08(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7210(19)
_cell_length_b                   14.384(3)
_cell_length_c                   17.153(3)
_cell_measurement_reflns_used    72684
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.999
_cell_measurement_theta_min      1.488
_cell_volume                     2334.0(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'CCD Detector'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20744
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.836
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.034
_exptl_transmission_factor_max   none
_exptl_transmission_factor_min   none
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0526
_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^)+(0.1030P)^2^+0.6520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9081
_reflns_number_total             10770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04809g2.cif
_cod_data_source_block           HCCP3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126981.cif.
;
_cod_original_cell_volume        2334.0(9)
_cod_original_formula_sum        'C43 H62.50 Cl Li N11.50 O7'
_cod_database_code               7126981
_shelx_shelxl_version_number     2014/7
_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, All O(H,H) groups
2. Others
 Fixed Sof: N57(0.5) C58(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
3.a Rotating group:
 O63(H63A,H63B), O64(H64A,H64B), O65(H65A,H65B)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C29(H29A,H29B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,
 H46B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B),
 C54(H54A,H54B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N11(H11), N17(H17), N23(H23), C3(H3), C4(H4), C8(H8), C9(H9),
 C14(H14), C15(H15), C20(H20), C21(H21), C37(H37), C42(H42)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C62(H62A,H62B,H62C), C59(H59A,
 H59B,H59C)
;
_shelx_res_checksum              13669
_olex2_submission_special_instructions 'No special instructions were received'