The <i>tert</i>-butylammonium perchlorate complex of 2,3-naphtho-18-crown-6 at 115K
Knobler, Carolyn B.; Maverick, Emily F.; Trueblood, Kenneth N.; Weiss, Robert M.; Acta Crystallographica Section C 55 (1999) 2091–2093; doi:10.1107/S010827019901080X

data_2009265
_publ_section_title
;
 The <i>tert</i>-butylammonium perchlorate complex of
 2,3-naphtho-18-crown-6 at 115K
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2091
_journal_page_last               2093
_journal_paper_doi               10.1107/S010827019901080X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety
'C4 H12 N^+^ , ClO4^-^ , C20 H26 O6 , 0.25C4 H8 O2 , 0.25C H2 Cl2'
_chemical_formula_sum            'C25.25 H40.5 Cl1.5 N O10.5'
_chemical_formula_weight         579.26
_chemical_name_common
;
naphthyl 18-crown-6 t-butyl ammonium perchlorate complex
;
_chemical_name_systematic
;
tert-butylammonium
perchlorate--2,5,8,11,14,17-hexaoxatricyclo[16.8.0.0^20,25^]hexacosa-
1(26),18,20(25),21,23-pentaene--ethyl acetate--dichloromethane (4/4/1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                102.36(2)
_cell_angle_beta                 111.79(2)
_cell_angle_gamma                100.28(2)
_cell_formula_units_Z            2
_cell_length_a                   10.996(3)
_cell_length_b                   11.423(3)
_cell_length_c                   13.501(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      12.76
_cell_measurement_theta_min      8.62
_cell_volume                     1474.7(7)
_computing_cell_refinement       'P\=1 software'
_computing_data_collection       'P\=1 software'
_computing_data_reduction        'UCLA Crystallographic Package (UCLA, 1984)'
_computing_molecular_graphics    'SHELXTL (Sheldrick 1995)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_measurement_device       'Syntex P\=1'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  'see Refinement'
_diffrn_reflns_av_sigmaI/netI    0.057
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7816
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             617
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.088
_refine_ls_R_factor_gt           0.074
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1728P)^2^+0.9323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.249
_refine_ls_wR_factor_ref         0.249
_reflns_number_gt                5547
_reflns_number_total             6812
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fr1227.cif
_cod_data_source_block           ntb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1728P)^2^+0.9323P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.1728P)^2^+0.9323P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C25.25 H40.50 Cl1.50 N O10.50'
_cod_database_code               2009265