Engineering N-(2-pyridyl)aminoethyl alcohols as potential precursors of thermolabile protecting groups
Chmielewski, Marcin K.; Tykarska, Ewa; Markiewicz, Wojciech T.; Rypniewski, Wojciech; New Journal of Chemistry 36 (2012) 603–; doi:10.1039/c1nj20584f

data_7052832
_publ_section_title
;
 Engineering N-(2-pyridyl)aminoethyl alcohols as potential precursors of
 thermolabile protecting groups
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              603
_journal_paper_doi               10.1039/c1nj20584f
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C12 H13 N3 O'
_chemical_formula_sum            'C12 H13 N3 O'
_chemical_formula_weight         215.25
_chemical_name_common            N-(2-pyrimidyl)amino-1-phenyloethanol
_chemical_name_systematic
;
N-(2-pyrimidyl)amino-1-phenyloethanol
;
_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_creation_method           SHELXL-97
_audit_update_record
;
2011-11-03 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6050(11)
_cell_length_b                   20.972(4)
_cell_length_c                   9.5000(19)
_cell_measurement_reflns_used    41067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.98
_cell_measurement_theta_min      2.82
_cell_volume                     1061.4(4)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MARCCD software'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows - Version 2.00, Univ. of Glasgow 2008.
Mercury CSD 2.3 - new features for the visualization and investigation
of crystal structures, C. F. Macrae, I. J. Bruno, J. A. Chisholm,
P. R. Edgington, P. McCabe, E. Pidcock, L. Rodriguez-Monge, R. Taylor,
J. van de Streek and P. A. Wood, J. Appl. Cryst., 41, 466-470, 2008.
;
_computing_publication_material  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'MARCCD 165mm'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Si111 single crystal'
_diffrn_radiation_source
;
EMBL beamline X13, HASYLAB, Hamburg, Germany.
;
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81620
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41074
_diffrn_reflns_theta_full        32.98
_diffrn_reflns_theta_max         32.98
_diffrn_reflns_theta_min         2.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.060(14)
_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_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0834P)^2^+0.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                2522
_reflns_number_total             2574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20584f.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052832