Separation of planar rotamers through intramolecular hydrogen bonding in polysubstituted 5-nitrosopyrimidines.
Čechová, L; Procházková, E; Císařová, I; Dračínský, M; Janeba, Z.; Chemical communications (Cambridge, England) 50 (2014) 14892–14895; doi:10.1039/c4cc06978a

data_7124581
_publ_section_title
;
 Separation of planar rotamers through intramolecular hydrogen bonding in
 polysubstituted 5-nitrosopyrimidines.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14892
_journal_page_last               14895
_journal_paper_doi               10.1039/c4cc06978a
_journal_volume                  50
_journal_year                    2014
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C11 H21 N6 O5 P, H2 O'
_chemical_formula_sum            'C11 H23 N6 O6 P'
_chemical_formula_weight         366.32
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-05-05 # Formatted by publCIF

;
_cell_angle_alpha                113.4116(10)
_cell_angle_beta                 92.8654(11)
_cell_angle_gamma                108.2169(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5829(2)
_cell_length_b                   10.4800(3)
_cell_length_c                   11.4529(3)
_cell_measurement_reflns_used    4983
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5332
_cell_measurement_theta_min      2.2722
_cell_volume                     879.87(4)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9450
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9763
_exptl_absorpt_correction_T_min  0.8789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0530P)^2^+0.6451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                3327
_reflns_number_total             3951
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc06978a6.cif
_cod_data_source_block           lc_190_etac_met_budes
_cod_database_code               7124581
_publcif_datablock.id            {d08afd2c-c488-49d6-9938-fd9686b8c9a8}