1,15:21,35-Bis(oxydiethylene)-5,8,11,18,25,28,31,38-octaoxa-1,15,21,35-tetraazacyclotetradecane-16,20,36,40-tetraone–benzene (1/2): a macrotricyclic tetralactam
Smith, Gary L. N.; Nguyen, Tam; Powell, Douglas R.; Taylor, Richard W.; Acta Crystallographica Section E 65 (2009) o1927–; doi:10.1107/S1600536809026531

data_2222832
_publ_section_title
;1,15:21,35-Bis(oxydiethylene)-5,8,11,18,25,28,31,38-octaoxa-1,15,21,35-tetraazacyclotetradecane-16,20,36,40-tetraone--benzene
 (1/2): a macrotricyclic tetralactam
;
_journal_coeditor_code           PK2175
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1927
_journal_paper_doi               10.1107/S1600536809026531
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C36 H64 N4 O14, 2C6 H6'
_chemical_formula_moiety         'C36 H64 N4 O14, 2(C6 H6)'
_chemical_formula_sum            'C48 H76 N4 O14'
_chemical_formula_weight         933.13
_chemical_name_systematic
;
1,15:21,35-Bis(oxydiethylene)-5,8,11,18,25,28,31,38-octaoxa-1,15,21,35-
tetraazacyclotetradecane-16,20,36,40-tetraone--benzene (1/2)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.728(5)
_cell_angle_beta                 71.758(5)
_cell_angle_gamma                68.443(6)
_cell_formula_units_Z            1
_cell_length_a                   8.9632(14)
_cell_length_b                   11.988(2)
_cell_length_c                   12.806(2)
_cell_measurement_reflns_used    7833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.26
_cell_volume                     1189.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       \w
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9363
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.211
_refine_ls_extinction_coef       0.0145(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^+0.42P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                4198
_reflns_number_total             4603
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2175.cif
_cod_data_source_block           I
_cod_database_code               2222832
_cod_database_fobs_code          2222832