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#$Date: 2016-03-26 02:58:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180163 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/59/7105953.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7105953
loop_
_publ_author_name
'Andrzej Katrusiak'
'Marek Szafranski'
'Marcin Podsiadlo'
_publ_section_title
;
 Pressure-induced collapse of guanidinium nitrate NâHâ ââO bonded
 honeycomb layers into a 3-D pattern with varied H-acceptor capacity
;
_journal_name_full               Chem.Commun.
_journal_page_first              2107
_journal_paper_doi               10.1039/c0cc02630a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C H6 N3, N O3'
_chemical_formula_sum            'C H6 N4 O3'
_chemical_formula_weight         122.10
_chemical_melting_point          486
_chemical_name_common            'guanidinium nitrate'
_chemical_name_systematic
;
guanidinium nitrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.340(3)
_cell_length_b                   7.2110(14)
_cell_length_c                   7.3900(15)
_cell_measurement_reflns_used    997
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.47
_cell_volume                     538.7(3)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         360000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.151
_diffrn_measured_fraction_theta_max 0.151
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            997
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.082
_refine_diff_density_min         -0.087
_refine_diff_density_rms         0.018
_refine_ls_extinction_coef       0.38(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0513
_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/[σ²(Fo²)+(0.0000P)²+1.0702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                82
_reflns_number_total             100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC02630A.TXT
_cod_data_source_block           azg_polymorphII_0.36GPa
_cod_original_cell_volume        538.67(19)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7105953
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.893(2) 0.0000 0.246(5) 0.060(3) Uiso 1 2 d S . .
N1 N 0.9817(19) 0.0000 0.221(5) 0.063(2) Uiso 1 2 d S . .
H11 H 1.0162 -0.1031 0.2196 0.075 Uiso 0.50 1 calc PR . .
H12 H 1.0102 0.1031 0.2049 0.075 Uiso 0.50 1 calc PR . .
N2 N 0.8520(13) 0.1480(6) 0.269(3) 0.067(2) Uiso 1 1 d . . .
H3 H 0.8864 0.2512 0.2677 0.080 Uiso 1 1 calc R . .
H2 H 0.7889 0.1477 0.2869 0.080 Uiso 1 1 calc R . .
N3 N 0.569(2) 0.0000 0.280(5) 0.070(2) Uiso 1 2 d S . .
O1 O 0.4454(19) 0.0000 0.227(5) 0.095(3) Uiso 1 2 d S . .
O2 O 0.6167(9) 0.1520(5) 0.284(2) 0.072(2) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 120.1(4) . 6 ?
N1 C1 N2 120.1(4) . . ?
N2 C1 N2 119.4(8) 6 . ?
N3 N3 O2 0(10) 1 1 ?
N3 N3 O2 0(10) 1 . ?
O2 N3 O2 0.0(6) 1 . ?
N3 N3 O2 0(10) 1 6 ?
O2 N3 O2 124.3(7) 1 6 ?
O2 N3 O2 124.3(7) . 6 ?
N3 N3 O1 0(10) 1 . ?
O2 N3 O1 117.2(7) 1 . ?
O2 N3 O1 117.2(7) . . ?
O2 N3 O1 117.2(7) 6 . ?
N3 O1 N3 0(3) 1 . ?
O2 O2 N3 0(10) 1 1 ?
O2 O2 N3 0(10) 1 . ?
N3 O2 N3 0(2) 1 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.206(9) . ?
C1 N2 1.236(6) 6 ?
C1 N2 1.236(6) . ?
N3 N3 0.00(14) 1 ?
N3 O2 1.240(5) 1 ?
N3 O2 1.240(5) . ?
N3 O2 1.240(5) 6 ?
N3 O1 1.336(17) . ?
O1 N3 1.336(17) 1 ?
O2 O2 0.00(2) 1 ?
O2 N3 1.240(5) 1 ?
