Neutral thioether and selenoether macrocyclic coordination to Group 1 cations (Li-Cs) - synthesis, spectroscopic and structural properties.
Champion, Martin J. D.; Levason, William; Pugh, David; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18748–18759; doi:10.1039/c5dt02583d

data_7036256
_publ_section_title
;
 Neutral thioether and selenoether macrocyclic coordination to Group 1
 cations (Li-Cs) - synthesis, spectroscopic and structural properties.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18748
_journal_page_last               18759
_journal_paper_doi               10.1039/c5dt02583d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C12 H24 Na O4 Se2'
_chemical_formula_sum            'C44 H36 B F24 Na O4 Se2'
_chemical_formula_weight         1276.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-30 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.603(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.7830(12)
_cell_length_b                   67.748(7)
_cell_length_c                   17.4535(18)
_cell_measurement_reflns_used    18479
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.3
_cell_volume                     15015(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
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'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      100(2)
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_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       84
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_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.962
_diffrn_source                   'Rotating Anode'
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_exptl_absorpt_correction_type   multi-scan
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'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             7584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.070
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_refine_diff_density_max         2.560
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.

 Owing to rotational disorder of some CF~3~ groups within the [BAr^F^]^-^ anion,
 certain C-F bond lengths needed to be restrained using the DFIX command in 
 order to retain sensible bond lengths. Additionally, owing to positional 
 disorder within the macrocyclic ligand, certain C-C and C-O bond lengths also
 had to be restrained using DFIX.

 Isotropic thermal parameter restraints were applied to some F and C atoms.
;
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         26208
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_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.998
_reflns_friedel_fraction_full    0.997
_reflns_friedel_fraction_max     0.997
_reflns_number_gt                20975
_reflns_number_total             26208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02583d1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7036247--7036257.cif.'
_cod_database_code               7036256
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