Physical organic studies and dynamic covalent chemistry of picolyl heterocyclic amino aminals
Ciou, Ji-Ming; Zhu, Hong-Feng; Chang, Chia-Wen; Chen, Jing-Yun; Lin, Ya-Fan; RSC Advances 10 (2020) 40421–40427; doi:10.1039/D0RA08527H

data_7241671
_publ_section_title
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 Physical organic studies and dynamic covalent chemistry of picolyl
 heterocyclic amino aminals
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_journal_issue                   66
_journal_name_full               'RSC Advances'
_journal_page_first              40421
_journal_page_last               40427
_journal_paper_doi               10.1039/D0RA08527H
_journal_volume                  10
_journal_year                    2020
_chemical_formula_sum            'C16 H16 N5'
_chemical_formula_weight         278.34
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_audit_update_record
;
2019-10-27 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8760(3)
_cell_length_b                   8.68900(10)
_cell_length_c                   19.6210(4)
_cell_measurement_reflns_used    21664
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2877.14(8)
_computing_cell_refinement       'Denzo-SMN & Scalepack'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Denzo-SMN & Scalepack'
_computing_molecular_graphics    SHELX
_computing_publication_material  SHELX
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f-\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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20084
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0926(87)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.129
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.1890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1778
_refine_ls_wR_factor_obs         0.1471
_reflns_number_observed          2245
_reflns_number_total             3263
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d0ra08527h3.cif
_cod_data_source_block           ic9369
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.1890P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.1890P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7241671