Benzo-21-crown-7-Based [1]Rotaxanes: Syntheses, X-ray Crystal Structures, and Dynamic Characteristics
Zhou, Qizhong; Wei, Peifa; Zhang, Yanyan; Yu, Yihua; Yan, Xuzhou; Organic Letters 15 (2013) 5350–; doi:10.1021/ol402607x

data_1512586
_publ_section_title
;
 Benzo-21-crown-7-Based [1]Rotaxanes: Syntheses, X-ray Crystal Structures,
 and Dynamic Characteristics
;
_journal_issue                   20
_journal_name_full               'Organic Letters'
_journal_page_first              5350
_journal_paper_doi               10.1021/ol402607x
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C51 H61 F6 N2 O13 P'
_chemical_formula_sum            'C51 H61 F6 N2 O13 P'
_chemical_formula_weight         1054.99
_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-97
_cell_angle_alpha                72.293(3)
_cell_angle_beta                 70.801(3)
_cell_angle_gamma                73.133(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7853(4)
_cell_length_b                   13.9375(5)
_cell_length_c                   17.3593(5)
_cell_measurement_reflns_used    5882
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.5539
_cell_measurement_theta_min      2.8259
_cell_volume                     2720.04(16)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18099
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.9588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9949
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2350
_refine_ls_wR_factor_ref         0.2588
_reflns_number_gt                6115
_reflns_number_total             9949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402607x_si_002.cif
_cod_data_source_block           1
_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 
;
_cod_original_cell_volume        2720.03(15)
_cod_database_code               1512586