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_7213309
_publ_section_title
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 The synthesis and structural characterization of the first bis(benzocrown
 ethers) with polyyne linkages&#x200A;&#x2020;
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_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            'C32 H38 O10'
_chemical_formula_weight         582.62
_chemical_name_systematic
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 Bis (benzo-15-crown-5) 1,3 butadiyne 
;
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.95(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.344(1)
_cell_length_b                   5.1406(5)
_cell_length_c                   21.862(3)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      10.9
_cell_measurement_theta_min      4.5
_cell_volume                     1472.3(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            2581
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.097
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       needle
_exptl_crystal_F_000             620
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0051(34)
_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   1.276
_refine_ls_goodness_of_fit_obs   1.620
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         1872
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.329
_refine_ls_restrained_S_obs      1.629
_refine_ls_R_factor_all          0.2049
_refine_ls_R_factor_obs          0.1143
_refine_ls_shift/esd_max         -0.368
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+4.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2671
_refine_ls_wR_factor_obs         0.2226
_reflns_number_observed          927
_reflns_number_total             1872
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001856msup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0492P)^2^+4.6057P] 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^)+(0.0492P)^2^+4.6057P] 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      P21/c
_cod_database_code               7213309