#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:53:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178922 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/51/4115145.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_4115145
loop_
_publ_author_name
'Colin A. Bremner'
'Michael Simpson'
'William T. A. Harrison'
_publ_section_title
;
 New Molecular Perovskites: Cubic C4N2H12.NH4Cl3.H2O and 2-H Hexagonal
 C6N2H14.NH4Cl3
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10960
_journal_page_last               10961
_journal_paper_doi               10.1021/ja027484e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '(C6, N2, H14) (N H4) Cl3'
_chemical_formula_sum            'C6 H18 Cl3 N3'
_chemical_formula_weight         238.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   16.1616(2)
_cell_length_b                   16.1616(2)
_cell_length_c                   22.3496(4)
_cell_measurement_reflns_used    18271
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5055.56(13)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
;
 DENZO (Otwinowski and Minor, 1997
 COLLECT (Hooft, 1998)
;
_computing_data_reduction        'DENZO and COLLECT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28403
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.967
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0034(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0978P)²+17.0285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2603
_reflns_number_gt                1719
_reflns_number_total             3856
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja027484e_s1_2.cif
_cod_data_source_block           hex
_cod_database_code               4115145
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x-y, -y, -z-1/2'
'-x, -x+y, -z-1/2'
'y, x, -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
Cl1 Cl 0.66163(10) 0.49597(9) 0.91563(6) 0.0283(4) Uani 1 1 d .
Cl2 Cl 0.30357(7) 0.48786(8) 0.75372(5) 0.0177(4) Uani 1 1 d .
Cl3 Cl 0.51545(9) 0.15626(9) 0.58874(5) 0.0234(4) Uani 1 1 d .
Cl4 Cl 0.0000 0.16529(10) 0.2500 0.0199(4) Uani 1 2 d S
Cl5A Cl 0.14943(12) -0.02920(15) 0.57706(6) 0.0169(6) Uani 0.817(7) 1 d P
Cl5B Cl 0.1799(6) 0.0325(7) 0.5768(3) 0.025(2) Uani 0.183(7) 1 d P
N1 N 0.0000 0.0000 0.3300(4) 0.040(2) Uani 1 3 d S
N2 N 0.0000 0.0000 1.0000 0.028(3) Uani 1 6 d S
N3 N 0.6667 0.3333 0.6663(4) 0.0341(19) Uani 1 3 d S
N4 N 0.6667 0.3333 0.8353(4) 0.040(2) Uani 1 3 d S
N5 N 0.6667 0.3333 0.4983(4) 0.043(3) Uani 1 3 d S
N10 N 0.9123(2) 0.2823(3) 0.74881(16) 0.0110(8) Uani 1 1 d .
H10 H 0.8459 0.2483 0.7483 0.013 Uiso 1 1 calc R
C1 C 0.9467(3) 0.2557(3) 0.69428(18) 0.0108(8) Uani 1 1 d .
H1A H 0.9247 0.2742 0.6579 0.013 Uiso 1 1 calc R
H1B H 0.9211 0.1858 0.6933 0.013 Uiso 1 1 calc R
C2 C 0.9449(3) 0.2530(3) 0.80364(18) 0.0114(8) Uani 1 1 d .
H2A H 0.9220 0.1837 0.8023 0.014 Uiso 1 1 calc R
H2B H 0.9183 0.2664 0.8399 0.014 Uiso 1 1 calc R
C3 C 0.9438(4) 0.3864(3) 0.7503(3) 0.0221(11) Uani 1 1 d .
H3A H 0.9197 0.4019 0.7868 0.026 Uiso 1 1 calc R
H3B H 0.9189 0.4039 0.7149 0.026 Uiso 1 1 calc R
N11 N 0.6151(4) 0.5798(4) 0.0848(2) 0.0328(12) Uani 1 1 d .
H11 H 0.5814 0.5133 0.0858 0.039 Uiso 1 1 calc R
N12 N 0.7063(3) 0.7575(3) 0.08207(19) 0.0215(9) Uani 1 1 d .
H12 H 0.7414 0.8239 0.0810 0.026 Uiso 1 1 calc R
C4 C 0.5874(4) 0.6088(4) 0.0305(2) 0.0332(14) Uani 1 1 d .
H4A H 0.5176 0.5840 0.0306 0.040 Uiso 1 1 calc R
H4B H 0.6031 0.5823 -0.0048 0.040 Uiso 1 1 calc R
C5 C 0.5927(4) 0.6130(4) 0.1400(2) 0.0321(13) Uani 1 1 d .
H5A H 0.6170 0.5942 0.1750 0.039 Uiso 1 1 calc R
H5B H 0.5227 0.5845 0.1442 0.039 Uiso 1 1 calc R
C6 C 0.7197(5) 0.6108(5) 0.0830(4) 0.0436(16) Uani 1 1 d .
H6A H 0.7379 0.5863 0.1182 0.052 Uiso 1 1 calc R
H6B H 0.7353 0.5873 0.0461 0.052 Uiso 1 1 calc R
C7 C 0.6411(4) 0.7183(4) 0.0271(3) 0.0308(12) Uani 1 1 d .
H7A H 0.6797 0.7400 -0.0100 0.037 Uiso 1 1 calc R
H7B H 0.5951 0.7418 0.0267 0.037 Uiso 1 1 calc R
C8 C 0.6412(4) 0.7233(4) 0.1363(2) 0.0300(12) Uani 1 1 d .
H8A H 0.5921 0.7425 0.1328 0.036 Uiso 1 1 calc R
H8B H 0.6788 0.7524 0.1731 0.036 Uiso 1 1 calc R
C9 C 0.7700(4) 0.7176(4) 0.0836(2) 0.0235(11) Uani 1 1 d .
H9A H 0.8098 0.7408 0.1202 0.028 Uiso 1 1 calc R
H9B H 0.8134 0.7420 0.0487 0.028 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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_3
C1 N10 C3 112.1(4) .
C1 N10 C2 109.8(3) .
C3 N10 C2 111.2(4) .
N10 C1 C2 107.9(3) 11_767
N10 C2 C1 108.6(3) 11_767
N10 C3 C3 107.1(2) 11_767
C4 N11 C5 114.4(5) .
C4 N11 C6 110.2(5) .
C5 N11 C6 110.1(5) .
C9 N12 C8 109.4(4) .
C9 N12 C7 109.1(4) .
C8 N12 C7 106.3(4) .
N11 C4 C7 109.0(4) .
N11 C5 C8 107.7(4) .
C9 C6 N11 104.8(5) .
N12 C7 C4 108.2(4) .
N12 C8 C5 108.7(4) .
N12 C9 C6 114.4(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl5A Cl5B 0.864(9) .
N10 C1 1.488(5) .
N10 C3 1.496(6) .
N10 C2 1.500(5) .
C1 C2 1.519(6) 11_767
C2 C1 1.519(6) 11_767
C3 C3 1.573(10) 11_767
N11 C4 1.451(8) .
N11 C5 1.460(7) .
N11 C6 1.504(8) .
N12 C9 1.462(7) .
N12 C8 1.517(7) .
N12 C7 1.534(7) .
C4 C7 1.534(8) .
C5 C8 1.549(8) .
C6 C9 1.496(8) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 Cl2 0.93 2.10 3.027(4) 174.5 11_657
N11 H11 Cl3 0.93 2.17 3.093(5) 174.8 5_554
N12 H12 Cl5A 0.93 2.06 2.990(5) 178.5 4_664
