An effective self-templating ring closure method for mixed donor thiophene-based macrocycles
Halfpenny, Joan; Sloman, Zachary S.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1877–; doi:10.1039/b002029j

data_7213317
_publ_section_title
;
 An effective self-templating ring closure method for mixed donor
 thiophene-based macrocycles
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1877
_journal_paper_doi               10.1039/b002029j
_journal_year                    2000
_chemical_formula_moiety         'C29 H32 N2 O2 S2'
_chemical_formula_sum            'C29 H32 N2 O2 S2'
_chemical_formula_weight         504.69
_chemical_melting_point          402.3(7)
_chemical_name_systematic
; 
 13,16--dibenzyl--2,6--dioxa--10,19--dithia--13,16--diazatricyclo
[16.3.0^7,11^]heneicosa--1^18^,20,7^11^,8--tetraene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.30(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.504(11)
_cell_length_b                   11.299(10)
_cell_length_c                   19.80(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     2569(5)
_computing_data_collection       'Stoe STADI--2'
_computing_data_reduction        'DATR (Small, 1977)'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
' MULTAN87 (Debaerdemaeker, Germain, Main, Tate and Woolfson, 1987)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Stoe STADI--2 two--circle diffractometer'
_diffrn_measurement_method
;
variable \w scan, 2\q' fixed, where the angle \q' is the projection 
of \q on the equatorial plane.
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine--focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7225
_diffrn_reflns_theta_full        29.79
_diffrn_reflns_theta_max         29.79
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        'maximum 5% corrected by interpolation'
_diffrn_standards_interval_count 20
_diffrn_standards_number         'one per layer'
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'PLATON (Spek, 1998)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      1.31
_exptl_crystal_density_method
;
flotation
;
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+0.3142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                2823
_reflns_number_total             7225
_reflns_threshold_expression     \\rangle2sigma(I)
_cod_data_source_file            b002029jsup1.cif
_cod_data_source_block           c3c2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '128.5--129.9 \%C' was changed to
'402.3(7)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2570(4)
_cod_original_sg_symbol_H-M      P2~1~/c
_cod_database_code               7213317