Competition Between the Donor and Acceptor Hydrogen Bonds of the Threads in the Formation of [2]Rotaxane by Clipping Reaction
Martins, Marcos A. P.; Zimmer, Geórgia Cristiane; Rodrigues, Leticia V.; Orlando, Tainára; Buriol, Lilian; Alajarin, Mateo; Berna, Jose; Frizzo, Clarissa Piccinin; Bonacorso, Helio Gauze; Zanatta, Nilo; New J. Chem. 41 (2017) 13303–13318; doi:10.1039/C7NJ02443F

data_7056659
_publ_section_title
;
 Competition Between the Donor and Acceptor Hydrogen Bonds of the Threads
 in the Formation of [2]Rotaxane by Clipping Reaction
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13303
_journal_page_last               13318
_journal_paper_doi               10.1039/C7NJ02443F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C31 H33 Cl N5 O4'
_chemical_formula_sum            'C31 H33 Cl N5 O4'
_chemical_formula_weight         575.07
_chemical_melting_point          'up 523K'
_chemical_name_common            rotaxane
_chemical_name_systematic
;
 ?
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2014-10-15T15:48:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-09-21 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                80.519(4)
_cell_angle_beta                 73.258(4)
_cell_angle_gamma                76.892(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6985(7)
_cell_length_b                   11.4602(9)
_cell_length_c                   14.9575(12)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.443
_cell_volume                     1541.7(2)
_computing_cell_refinement       'BRUKER SANT'
_computing_data_collection       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER SOFTWARE'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'X8 APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43020
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP (Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.1699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                5116
_reflns_number_total             6748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02443f2.cif
_cod_data_source_block           compound_10e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7056659
_exptl_absorpt_special_details
;
 XPREP (Bruker, 2006) was used to perform the Gaussian absorption
        correction based on the face-indexed crystal size
;