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_7056662
_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         'C30 H36 N6 O2'
_chemical_formula_sum            'C30 H36 N6 O2'
_chemical_formula_weight         512.65
_chemical_melting_point          ?
_chemical_name_common            thread-1,5-fenil
_chemical_name_systematic
;
'1,2-bis(aminocarbonyl-(3'-phenyl)-(1'(tert-butyl)-1H-pyrazole-5'-il)ethane'
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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      2.4
_audit_creation_date             2017-04-08T09:48:19-00:00
_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                90
_cell_angle_beta                 100.744(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0096(10)
_cell_length_b                   18.5432(14)
_cell_length_c                   12.0412(9)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.089
_cell_measurement_theta_min      4.2025
_cell_volume                     2853.9(4)
_computing_cell_refinement       'BRUKER SANT'
_computing_data_collection       'BRUKER APEX-III'
_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, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22676
_diffrn_reflns_theta_full        68.18
_diffrn_reflns_theta_max         68.18
_diffrn_reflns_theta_min         4.2
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1612P)^2^+5.3603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3381
_refine_ls_wR_factor_ref         0.3454
_reflns_number_gt                4506
_reflns_number_total             5035
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7nj02443f2.cif
_cod_data_source_block           compound_8c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

'_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     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7056662
_exptl_absorpt_special_details
;
'SADABS (version 2012/1; Bruker, 2012) was used to perform the numerical
absorption correction based on the indexed faces of the cystal.'
;