(1,4,7,10-Tetraoxacyclododecane)(trideuteroacetonitrile)lithium perchlorate
Guzei, Ilia A.; Spencer, Lara C.; Xiao, Lingyun; Burnette, Ronald R.; Acta Crystallographica Section E 66 (2010) m440–m441; doi:10.1107/S1600536810009530

data_2225694
_publ_section_title
;
 (1,4,7,10-Tetraoxacyclododecane)(trideuteroacetonitrile)lithium
 perchlorate
;
_journal_coeditor_code           SI2247
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m440
_journal_page_last               m441
_journal_paper_doi               10.1107/S1600536810009530
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Li (C8 H16 O4) (C2 D3 N)] Cl O4'
_chemical_formula_moiety         'C10 H16 D3 Li N O4 +, Cl O4 -'
_chemical_formula_sum            'C10 H16 Cl D3 Li N O8'
_chemical_formula_weight         323.65
_chemical_name_systematic
;
(1,4,7,10-Tetraoxacyclododecane)(trideuteroacetonitrile)lithium perchlorate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.1605(14)
_cell_length_b                   12.6338(15)
_cell_length_c                   19.870(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.54
_cell_volume                     3052.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), <i>publCIF</i> (Westrip, 2010) and
<i>modiCIFer</i>
(Guzei, 2007)
;
_computing_structure_refinement
'SHELXTL (Sheldrick, 2008) and <i>FCF_filter</i> (Guzei, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker CCD-1000 area-detector'
_diffrn_measurement_method       '0.30\% \w and 0.4 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20941
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9452
_exptl_absorpt_correction_T_min  0.8946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+6.1747P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                2164
_reflns_number_total             2621
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2247.cif
_cod_data_source_block           I
_cod_database_code               2225694
_cod_database_fobs_code          2225694