Synthesis of a double-spanned resorc[4]arene via ring-closing metathesis and calculation of aggregation propensity.
Ghirga, Francesca; Quaglio, Deborah; Iovine, Valentina; Botta, Bruno; Pierini, Marco; Mannina, Luisa; Sobolev, Anatoly P.; Ugozzoli, Franco; D'Acquarica, Ilaria; The Journal of organic chemistry 79 (2014) 11051–11060; doi:10.1021/jo502056v

data_4030143
_publ_section_title
;
 Synthesis of a double-spanned resorc[4]arene via ring-closing metathesis
 and calculation of aggregation propensity.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11051
_journal_page_last               11060
_journal_paper_doi               10.1021/jo502056v
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C84 H120 O16'
_chemical_formula_weight         1385.80
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.919(5)
_cell_angle_beta                 111.026(5)
_cell_angle_gamma                81.180(5)
_cell_formula_units_Z            2
_cell_length_a                   15.775(5)
_cell_length_b                   22.923(5)
_cell_length_c                   12.270(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      20
_cell_volume                     4059(2)
_computing_cell_refinement       'DIPCHIGE software package 2004'
_computing_data_collection       'DIPCHIGE software package 2004'
_computing_data_reduction        DIFAU92
_computing_molecular_graphics    'Accelrys DS-ViewerPro 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (C. Giacovazzo et. al. 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 1KeV
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens AED'
_diffrn_measurement_method       'Scintil counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0065
_diffrn_reflns_av_sigmaI/netI    0.1661
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_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            14493
_diffrn_reflns_theta_full        65.03
_diffrn_reflns_theta_max         65.03
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  1.11
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick column'
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.269
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         13777
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      0.800
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                3448
_reflns_number_total             13777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502056v_si_002.cif
_cod_data_source_block           bsk
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4030143.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4030143