Internal and External Stereoisomers of Squaraine Rotaxane Endoperoxide: Synthesis, Chemical Differences, and Structural Revision.
Collins, Carleton G.; Lee, Joshua M.; Oliver, Allen G.; Wiest, Olaf; Smith, Bradley D.; The Journal of organic chemistry 79 (2014) 1120–; doi:10.1021/jo402564k

data_4029033
_publ_section_title
;
 Internal and External Stereoisomers of Squaraine Rotaxane Endoperoxide:
 Synthesis, Chemical Differences, and Structural Revision.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1120
_journal_paper_doi               10.1021/jo402564k
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C56 H52 N4 O6, C4 H8 O, C H4 O, 0.5(H2 O)'
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_chemical_name_systematic
;
 ?
;
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   difmap
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_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      3.56
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_computing_data_reduction        'Bruker SAINT v8.18C'
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_diffrn_ambient_temperature      120(2)
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_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
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_diffrn_reflns_av_unetI/netI     0.0260
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_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            91109
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
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_diffrn_reflns_theta_max         71.578
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'Incoatec micro-focus'
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_exptl_absorpt_correction_T_min  0.9206
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_exptl_crystal_description       needle
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_exptl_crystal_size_min          0.04
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_refine_ls_number_reflns         9624
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+3.9182P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7580
_reflns_number_total             9624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo402564k_si_002.cif
_cod_data_source_block           nd1301a
_cod_original_formula_sum        'C61 H65 N4 O8.50'
_cod_database_code               4029033
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelxl_version_number           2012-6