Two related lithium calixarene complexes, [<i>p-tert</i>-butylcalix[4]arene(OMe)(OH)~2~(OLi)]~2~·4MeCN and {<i>p-tert</i>-butylcalix[4]arene(OH)~2~(OLi)[OLi(NCMe)~2~]}~2~·8MeCN, determined using synchrotron radiation
Lee, Darren S.; Elsegood, Mark R. J.; Redshaw, Carl; Zhan, Shuzhong; Acta Crystallographica Section C 65 (2009) m291–m295; doi:10.1107/S0108270109025311

data_2017214
_publ_section_title
;Two related lithium calixarene complexes,
 [<i>p-tert</i>-butylcalix[4]arene(OMe)(OH)~2~(OLi)]~2~&#x00B7;4MeCN and
 {<i>p-tert</i>-butylcalix[4]arene(OH)~2~(OLi)[OLi(NCMe)~2~]}~2~&#x00B7;8MeCN,
 determined using synchrotron radiation
;
_journal_coeditor_code           EG3021
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m291
_journal_page_last               m295
_journal_paper_doi               10.1107/S0108270109025311
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Li4 (C44 H54 O4)2 (C2 H3 N)4], 8C2 H3 N'
_chemical_formula_moiety         'C96 H120 Li4 N4 O8, 8(C2 H3 N)'
_chemical_formula_sum            'C112 H144 Li4 N12 O8'
_chemical_formula_weight         1814.16
_chemical_name_common
;
{<i>p-tert</i>-butylcalix[4]arene(OH)~2~(OLi)[OLi(NCMe)~2~]}~2~.8MeCN
;
_chemical_name_systematic
;
Tetraacetonitrilebis(\m-5,11,17,23-tetra-<i>tert</i>-butyl-26,28-dihydroxy-
25,27-dioxidocalix[4]arene)tetralithium(I) acetonitrile octasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except H2 and H4 coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.035(2)
_cell_angle_beta                 94.097(2)
_cell_angle_gamma                115.286(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8190(12)
_cell_length_b                   13.5649(13)
_cell_length_c                   18.223(3)
_cell_measurement_reflns_used    1271
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      3.73
_cell_volume                     2687.5(6)
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Version 6.10; Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Version 6.10; Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2SMX'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8466
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15630
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Version 2.10; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.239
_refine_ls_extinction_coef       0.0042(8)
_refine_ls_extinction_expression
Fc\^*\^=kFc[1+0.001xFc\^2\^\l\^3\^/sin(2\q)]\^-1/4\^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         7870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[\s\^2\^(Fo\^2\^)+(0.0771P)\^2\^+0.0000P] where
 P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1717
_reflns_number_gt                4532
_reflns_number_total             7870
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3021.cif
_cod_data_source_block           II
_cod_original_cell_volume        2687.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017214
_cod_database_fobs_code          2017214