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_2017213
_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          '[Li2 (C45 H57 O4)2], 4C2 H3 N'
_chemical_formula_moiety         'C90 H114 Li2 O8, 4(C2 H3 N)'
_chemical_formula_sum            'C98 H126 Li2 N4 O8'
_chemical_formula_weight         1501.91
_chemical_name_common
;
[<i>p-tert</i>-butylcalix[4]arene(OMe)(OH)~2~(OLi)]~2~.4MeCN
;
_chemical_name_systematic
;
bis(\m-5,11,17,23-tetra-<i>tert</i>-butyl-26,28-dihydroxy-25-methoxy-27-
oxidocalix[4]arene)dilithium(I) acetonitrile tetrasolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom except OH coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.2746(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8368(11)
_cell_length_b                   17.8044(15)
_cell_length_c                   19.6735(16)
_cell_measurement_reflns_used    5608
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.30
_cell_volume                     4496.4(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6911
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29080
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Version 2004/1; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8536
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+3.2181P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2258
_reflns_number_gt                5918
_reflns_number_total             8536
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3021.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017213
_cod_database_fobs_code          2017213