Two Macrocyclic Azacrown Ethers
Alessandra Forni; Acta Crystallographica Section C 54 (1998) 1921–1923; doi:10.1107/S0108270198007550

data_2007981
_publ_section_title
;
 Two Macrocyclic Azacrown Ethers
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1921
_journal_page_last               1923
_journal_paper_doi               10.1107/S0108270198007550
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C60 H68 N4 O4 , 2C H2 Cl2'
_chemical_formula_structural     'C60 H68 N4 O4 , 2C H2 Cl2'
_chemical_formula_sum            'C62 H72 Cl4 N4 O4'
_chemical_formula_weight         1079.04
_chemical_name_systematic
;
 4,10,16,22-tetra(1-naphthylmethyl)-1,7,13,19-tetraoxa-4,10,16,22-
 tetraazacyclotetracosano
;
_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                64.42(2)
_cell_angle_beta                 72.89(2)
_cell_angle_gamma                73.37(2)
_cell_formula_units_Z            1
_cell_length_a                   11.369(3)
_cell_length_b                   12.175(3)
_cell_length_c                   12.268(3)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    245(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      0
_cell_volume                     1438.7(7)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ZORTEP (Zsolnai & Pritzkow, 1995)'
_computing_publication_material
;
SHELXL93, PARST (Nardelli, 1983, 1995), PARSTCIF (Nardelli, 1991)
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      245(2)
_diffrn_measurement_device
;
Siemens SMART CCD with LT-2 device for low-temperature collection
;
_diffrn_measurement_method       frame
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13318
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.948
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment
;
H atoms of  CH~2~Cl~2~ riding; coordinates of remaining H atoms refined,
with U~iso~ restrained
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         5061
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.994
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_obs          0.0355
_refine_ls_shift/esd_max         -0.094
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0952
_refine_ls_wR_factor_obs         0.0840
_reflns_number_observed          3535
_reflns_number_total             5063
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1370.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0533P)^2^] 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^)+(0.0533P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1438.7(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2007981