Improved Synthesis of Larger Resorcinarenes.
Della Sala, Paolo; Gaeta, Carmine; Navarra, Wanda; Talotta, Carmen; De Rosa, Margherita; Brancatelli, Giovanna; Geremia, Silvano; Capitelli, Francesco; Neri, Placido; The Journal of organic chemistry 81 (2016) 5726–5731; doi:10.1021/acs.joc.6b00803

data_4032023
_publ_section_title
;
 Improved Synthesis of Larger Resorcinarenes.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5726
_journal_page_last               5731
_journal_paper_doi               10.1021/acs.joc.6b00803
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C60 H72 O12'
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_symmetry_cell_setting           monoclinic
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_audit_creation_method           'WinGX routine CIF_UPDATE'
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_cell_angle_gamma                90
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_cell_length_c                   25.7680(1)
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_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
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_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.2
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_refine_ls_extinction_coef       0.117(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.058
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.4354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             11185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00803_si_004.cif
_cod_data_source_block           prova
_cod_original_cell_volume        5219.9(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4032023
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              15225
_shelx_hkl_checksum              53082