Crystal structure of a supramolecular lithium complex of <i>p</i>-<i>tert</i>-butylcalix[4]arene
Yamada, Manabu; Gandhi, Muniyappan Rajiv; Akimoto, Kazuhiko; Hamada, Fumio; Acta Crystallographica Section E 74 (2018) 575–579; doi:10.1107/S2056989018001834

data_2242477
_publ_section_title
;
 Crystal structure of a supramolecular lithium complex of
 <i>p</i>-<i>tert</i>-butylcalix[4]arene
;
_journal_coeditor_code           XI2008
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              575
_journal_page_last               579
_journal_paper_doi               10.1107/S2056989018001834
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Li (C H3 O H)4] (C44 H55 O4), C H3 O H'
_chemical_formula_moiety         'Li C4 H16 O4 +, C44 H55 O4 -, C H3 OH'
_chemical_formula_sum            'C49 H75 Li O9'
_chemical_formula_weight         815.03
_chemical_name_systematic
'Tetramethanollithium 5,11,17,23-tetra-<i>tert</i>-butyl-25,26,27-trihydroxy-28-oxidocalix[4]arene methanol monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.561(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8434(4)
_cell_length_b                   20.0919(6)
_cell_length_c                   19.3168(6)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    200
_cell_measurement_theta_max      63.83
_cell_measurement_theta_min      3.18
_cell_volume                     4979.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2006)
;
_computing_data_collection
;
APEX2 (Bruker, 2006)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2006)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
;
<i>Yadokari-XG</i> (Kabuto <i>et al.</i>,  2009) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41849
_diffrn_reflns_theta_full        65.009
_diffrn_reflns_theta_max         65.009
_diffrn_reflns_theta_min         3.175
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker 2006)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plane
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1063P)^2^+3.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                6715
_reflns_number_total             8251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xi2008sup1.cif
_cod_data_source_block           I
_cod_database_code               2242477
_shelx_hkl_checksum              36418
_shelx_res_checksum              35043
_cod_database_fobs_code 2242477