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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/7/10/59/7105954.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_7105954
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           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 100.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.8990(10)
_cell_length_b                   4.9170(10)
_cell_length_c                   10.350(2)
_cell_measurement_reflns_used    1866
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      4.14
_cell_volume                     244.90(9)
_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         680000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.276
_diffrn_measured_fraction_theta_max 0.276
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1866
_diffrn_reflns_theta_full        28.93
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         4.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.26
_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    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.098
_refine_diff_density_min         -0.112
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(6)
_refine_ls_extinction_coef       0.48(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         350
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0669
_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+0.2119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                286
_reflns_number_total             350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC02630A.TXT
_cod_data_source_block           azg_polymorphIV_0.68GPa
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7105954
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
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 -0.209(4) 0.1069(13) 0.048(2) 0.0291(17) Uiso 1 1 d . . .
N1 N -0.325(2) 0.3244(10) 0.0059(13) 0.0363(15) Uiso 1 1 d . . .
H12 H -0.2651 0.4149 -0.0541 0.044 Uiso 1 1 calc R . .
H11 H -0.4656 0.3831 0.0367 0.044 Uiso 1 1 calc R . .
N2 N -0.262(3) -0.0026(12) 0.1497(15) 0.042(2) Uiso 1 1 d . . .
H21 H -0.1631 -0.1369 0.1853 0.051 Uiso 1 1 calc R . .
H22 H -0.3980 0.0562 0.1838 0.051 Uiso 1 1 calc R . .
N3 N -0.008(3) -0.0096(12) 0.0175(18) 0.050(2) Uiso 1 1 d . . .
H31 H 0.0698 -0.1431 0.0641 0.061 Uiso 1 1 calc R . .
H32 H 0.0547 0.0426 -0.0508 0.061 Uiso 1 1 calc R . .
N4 N 0.234(3) -0.5580(14) 0.2656(16) 0.037(2) Uiso 1 1 d . . .
O1 O 0.026(3) -0.4480(11) 0.3220(14) 0.0534(19) Uiso 1 1 d . . .
O2 O 0.276(3) -0.4662(11) 0.1779(13) 0.0409(17) Uiso 1 1 d . . .
O3 O 0.361(3) -0.7565(8) 0.3274(13) 0.0411(13) 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
N3 C1 N2 108.7(9) . . ?
N3 C1 N1 130(2) . . ?
N2 C1 N1 121(2) . . ?
C1 N1 H12 120.0 . . ?
C1 N1 H11 120.0 . . ?
H12 N1 H11 120.0 . . ?
C1 N2 H21 120.0 . . ?
C1 N2 H22 120.0 . . ?
H21 N2 H22 120.0 . . ?
C1 N3 H31 120.0 . . ?
C1 N3 H32 120.0 . . ?
H31 N3 H32 120.0 . . ?
N4 N4 N4 0(10) 1 1 ?
N4 N4 O2 0(10) 1 . ?
N4 N4 O2 0(10) 1 . ?
N4 N4 O2 0(10) 1 1 ?
N4 N4 O2 0(10) 1 1 ?
O2 N4 O2 0.0(18) . 1 ?
N4 N4 O3 0(10) 1 . ?
N4 N4 O3 0(10) 1 . ?
O2 N4 O3 127(2) . . ?
O2 N4 O3 127(2) 1 . ?
N4 N4 O1 0(10) 1 . ?
N4 N4 O1 0(10) 1 . ?
O2 N4 O1 118.1(10) . . ?
O2 N4 O1 118.1(10) 1 . ?
O3 N4 O1 115.1(17) . . ?
N4 N4 O1 0(10) 1 1 ?
N4 N4 O1 0(10) 1 1 ?
O2 N4 O1 118.1(10) . 1 ?
O2 N4 O1 118.1(10) 1 1 ?
O3 N4 O1 115.1(17) . 1 ?
O1 N4 O1 0.0(15) . 1 ?
O1 O1 N4 0(10) 1 1 ?
O1 O1 N4 0(10) 1 . ?
N4 O1 N4 0.0(13) 1 . ?
O1 O1 N4 0(10) 1 1 ?
N4 O1 N4 0.0(13) 1 1 ?
N4 O1 N4 0.0(13) . 1 ?
O2 O2 N4 0(10) 1 1 ?
O2 O2 N4 0(10) 1 . ?
N4 O2 N4 0.0(15) 1 . ?
O2 O2 N4 0(10) 1 1 ?
N4 O2 N4 0.0(15) 1 1 ?
N4 O2 N4 0.0(15) . 1 ?
N4 O3 N4 0.0(8) 1 . ?
N4 O3 N4 0.0(8) 1 1 ?
N4 O3 N4 0.0(8) . 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 N3 1.23(4) . ?
C1 N2 1.25(4) . ?
C1 N1 1.253(9) . ?
N1 H12 0.8600 . ?
N1 H11 0.8600 . ?
N2 H21 0.8600 . ?
N2 H22 0.8600 . ?
N3 H31 0.8600 . ?
N3 H32 0.8600 . ?
N4 N4 0.00(2) 1 ?
N4 N4 0.00(2) 1 ?
N4 O2 1.07(3) . ?
N4 O2 1.07(3) 1 ?
N4 O3 1.266(8) . ?
N4 O1 1.37(3) . ?
N4 O1 1.37(3) 1 ?
O1 O1 0.00(3) 1 ?
O1 N4 1.37(3) 1 ?
O1 N4 1.37(3) 1 ?
O2 O2 0.00(3) 1 ?
O2 N4 1.07(3) 1 ?
O2 N4 1.07(3) 1 ?
O3 N4 1.266(8) 1 ?
O3 N4 1.266(8) 1 ?
