The synthesis and structural characterization of the first bis(benzocrown ethers) with polyyne linkages †
Lee, Liang-Hui; Lynch, Vincent; Lagow, Richard J.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 2805–; doi:10.1039/b001856m

data_7213308
_publ_section_title
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 The synthesis and structural characterization of the first bis(benzocrown
 ethers) with polyyne linkages&#x200A;&#x2020;
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2805
_journal_paper_doi               10.1039/b001856m
_journal_year                    2000
_chemical_formula_sum            'C36 H38 O10'
_chemical_formula_weight         630.66
_chemical_name_systematic
; 
 Bis (benzo-15-crown-5) 1,3,5,7 octatetrayne
;
_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
_cell_angle_alpha                79.22(4)
_cell_angle_beta                 79.78(4)
_cell_angle_gamma                73.48(3)
_cell_formula_units_Z            2
_cell_length_a                   8.781(4)
_cell_length_b                   8.807(4)
_cell_length_c                   21.478(14)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      10.9
_cell_measurement_theta_min      5.1
_cell_volume                     1550.6(15)
_computing_cell_refinement       'XSCANS v2.10b, Siemens Analytical'
_computing_data_collection       'XSCANS v2.10b, Siemens Analytical'
_computing_data_reduction        'XSCANS v2.10b, Siemens Analytical'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4 '
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_sigmaI/netI    0.2364
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4261
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.44
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0131(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.282
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      0.996
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.2412
_refine_ls_R_factor_obs          0.0933
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2061
_refine_ls_wR_factor_obs         0.1473
_reflns_number_observed          1558
_reflns_number_total             4001
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001856msup1.cif
_cod_data_source_block           5
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.0292P] 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^)+(0.0496P)^2^+1.0292P] 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        1550.6(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213308