Hemispherand-Strapped Calix[4]pyrrole: An Ion-pair Receptor for the Recognition and Extraction of Lithium Nitrite.
He, Qing; Zhang, Zhan; Brewster, James T.; Lynch, Vincent M.; Kim, Sung Kuk; Sessler, Jonathan L.; Journal of the American Chemical Society 138 (2016) 9779–9782; doi:10.1021/jacs.6b05713

data_4130670
_publ_section_title
;
 Hemispherand-Strapped Calix[4]pyrrole: An Ion-pair Receptor for the
 Recognition and Extraction of Lithium Nitrite.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9779
_journal_page_last               9782
_journal_paper_doi               10.1021/jacs.6b05713
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C50 H58 Li N8 O5, 2(C H4 O), C2 H3 N, Cl'
_chemical_formula_sum            'C54 H69 Cl Li N9 O7'
_chemical_formula_weight         998.57
_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
_audit_creation_date             2016-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                85.376(11)
_cell_angle_beta                 88.134(14)
_cell_angle_gamma                89.723(11)
_cell_formula_units_Z            2
_cell_length_a                   10.850(5)
_cell_length_b                   13.688(6)
_cell_length_c                   18.213(8)
_cell_measurement_reflns_used    15033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0547
_cell_measurement_theta_min      1.1223
_cell_volume                     2695(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.1410
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39913
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.250
_diffrn_reflns_theta_min         1.493
_exptl_absorpt_coefficient_mu    0.130
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         15033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.1971
_refine_ls_R_factor_gt           0.1309
_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^)+(0.1008P)^2^+1.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.3001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9355
_reflns_number_total             15033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05713_si_002.cif
_cod_data_source_block           11
_cod_database_code               4130670
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.036) H3(0.037) H7(0.035) H8(0.033) H12(0.035) H13(0.034)
 H17(0.039) H18(0.038) H21A(0.046) H21B(0.046) H21C(0.046) H22A(0.044)
 H22B(0.044) H22C(0.044) H23A(0.043) H23B(0.043) H23C(0.043) H24A(0.047)
 H24B(0.047) H24C(0.047) H25A(0.048) H25B(0.048) H25C(0.048) H26A(0.041)
 H26B(0.041) H26C(0.041) H27A(0.03) H27B(0.03) H28A(0.037) H28B(0.037)
 H31(0.035) H32(0.041) H33(0.038) H36(0.038) H37(0.039) H38(0.036) H42(0.035)
 H43(0.04) H44(0.034) H47A(0.038) H47B(0.038) H48A(0.032) H48B(0.032)
 H49A(0.072) H49B(0.072) H49C(0.072) H50A(0.098) H50B(0.098) H50C(0.098)
 H51A(0.078) H51B(0.078) H51C(0.078) H52A(0.063) H52B(0.063) H52C(0.063)
 H54A(0.067) H54B(0.067) H54C(0.067) H4(0.03) H8A(0.034) H6(0.072)
 Fixed X: H2(0.4828) H3(0.5181) H7(0.301) H8(0.071) H12(-0.1923) H13(-0.2257)
 H17(-0.0389) H18(0.1875) H21A(0.5993) H21B(0.5103) H21C(0.4956) H22A(-0.0862)
 H22B(-0.2) H22C(-0.1371) H23A(0.0486) H23B(-0.0947) H23C(0.0046) H24A(-0.2174)
 H24B(-0.2778) H24C(-0.1933) H25A(0.403) H25B(0.3978) H25C(0.5143) H26A(0.4937)
 H26B(0.379) H26C(0.366) H27A(0.4545) H27B(0.4033) H28A(0.6157) H28B(0.6524)
 H31(0.7746) H32(0.8018) H33(0.7266) H36(0.7691) H37(0.6919) H38(0.4816)
 H42(0.2599) H43(0.051) H44(-0.0331) H47A(-0.0888) H47B(0.0525) H48A(-0.1476)
 H48B(-0.0066) H49A(0.3142) H49B(0.2948) H49C(0.4246) H50A(0.6351) H50B(0.6611)
 H50C(0.5276) H51A(0.0258) H51B(0.1237) H51C(-0.008) H52A(0.6232) H52B(0.6029)
 H52C(0.5355) H54A(0.0889) H54B(0.1273) H54C(0.2054) H4(0.1588) H8A(0.1545)
 H6(0.1272)
 Fixed Y: H2(1.0389) H3(1.0276) H7(0.9669) H8(0.9378) H12(0.9371) H13(0.9323)
 H17(0.9305) H18(0.9788) H21A(0.8915) H21B(0.874) H21C(0.9708) H22A(0.7955)
 H22B(0.7766) H22C(0.8825) H23A(0.6487) H23B(0.6377) H23C(0.648) H24A(0.8754)
 H24B(0.7712) H24C(0.784) H25A(1.0005) H25B(0.9124) H25C(0.9235) H26A(0.7571)
 H26B(0.7377) H26C(0.7186) H27A(0.7079) H27B(0.7034) H28A(0.7787) H28B(0.7243)
 H31(0.4251) H32(0.2582) H33(0.1962) H36(0.2528) H37(0.2012) H38(0.2133)
 H42(0.1269) H43(0.1516) H44(0.3092) H47A(0.6472) H47B(0.6542) H48A(0.6318)
 H48B(0.6462) H49A(0.1903) H49B(0.2641) H49C(0.21) H50A(0.5043) H50B(0.6145)
 H50C(0.5673) H51A(0.3276) H51B(0.3786) H51C(0.4285) H52A(0.5644) H52B(0.481)
 H52C(0.5849) H54A(-0.0452) H54B(-0.0291) H54C(0.0216) H4(0.7692) H8A(0.5177)
 H6(0.4992)
 Fixed Z: H2(0.1779) H3(0.315) H7(0.506) H8(0.5264) H12(0.3781) H13(0.241)
 H17(0.0488) H18(0.0283) H21A(0.4231) H21B(0.4948) H21C(0.4403) H22A(0.5528)
 H22B(0.502) H22C(0.4979) H23A(0.4182) H23B(0.4409) H23C(0.5029) H24A(0.1216)
 H24B(0.1472) H24C(0.0734) H25A(0.0669) H25B(0.0144) H25C(0.0647) H26A(0.122)
 H26B(0.0722) H26C(0.1599) H27A(0.4507) H27B(0.3697) H28A(0.3322) H28B(0.4095)
 H31(0.4558) H32(0.4389) H33(0.3323) H36(0.1756) H37(0.0683) H38(0.0466)
 H42(0.1206) H43(0.0948) H44(0.0883) H47A(0.0596) H47B(0.0815) H48A(0.1889)
 H48B(0.2082) H49A(0.2892) H49B(0.3525) H49C(0.3422) H50A(0.0205) H50B(0.0391)
 H50C(0.0562) H51A(0.3367) H51B(0.2783) H51C(0.2912) H52A(0.6223) H52B(0.5671)
 H52C(0.5537) H54A(0.2526) H54B(0.3348) H54C(0.2661) H4(0.1905) H8A(0.111)
 H6(0.3529)
;
_shelx_res_checksum              43448
_shelx_hkl_checksum              78603
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'