#------------------------------------------------------------------------------
#$Date: 2017-03-05 06:37:24 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193707 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/96/7119629.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_7119629
loop_
_publ_author_name
'Neudert, Lukas'
'Heinke, Frank'
'Bräuniger, Thomas'
'Pucher, Florian J.'
'Vaughan, Gavin B.'
'Oeckler, Oliver'
'Schnick, Wolfgang'
_publ_section_title
;
 An unusual nitride network of aluminum-centered octahedra and
 phosphorus-centered tetrahedra and structure determination from
 microcrystalline samples.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2709
_journal_page_last               2712
_journal_paper_doi               10.1039/c7cc00233e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'Al H2 N11 O P6'
_chemical_formula_sum            'Al H2 N11 O P6'
_chemical_formula_weight         384.93
_chemical_name_common            'aluminium oxonitridoimidophosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.601(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.7566(2)
_cell_length_b                   8.3266(3)
_cell_length_c                   10.6298(7)
_cell_measurement_reflns_used    2739
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18.41
_cell_measurement_theta_min      2.05
_cell_volume                     412.41(4)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       manual
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Diamond 3.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 CCD
_diffrn_detector_type            FReLoN2k
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Huber goniometer'
_diffrn_measurement_method       oscillation
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3351
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3577
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        11.599
_diffrn_reflns_theta_max         13.846
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'ESRF beamline ID11'
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.100
_exptl_crystal_description       platelet
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.007
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.0004
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0205P)²+0.1217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1103
_reflns_number_total             1285
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc00233e2.cif
_cod_data_source_block           AlPONH
_cod_depositor_comments          'Adding full bibliography for 7119629.cif.'
_cod_database_code               7119629
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
P1 P 0.16554(8) 0.08551(4) 0.32927(5) 0.00890(12) Uani 1 1 d . . .
P2 P 0.33412(8) 0.08486(4) 0.67156(5) 0.00893(12) Uani 1 1 d . . .
P3 P 0.10774(12) 0.2500 0.08409(7) 0.01196(14) Uani 1 2 d S T P
P4 P 0.53473(12) 0.2500 0.91759(7) 0.01218(15) Uani 1 2 d S T P
Al5 Al 0.75102(12) 0.2500 0.50031(7) 0.00978(16) Uani 1 2 d S T P
O1 O 0.4273(4) 0.2500 0.0511(2) 0.0218(5) Uani 0.52(3) 2 d S T P
N1 N 0.4273(4) 0.2500 0.0511(2) 0.0218(5) Uani 0.48(3) 2 d S T P
N2 N 0.8816(4) 0.2500 0.9501(2) 0.0225(5) Uani 0.52(3) 2 d S T P
O2 O 0.8816(4) 0.2500 0.9501(2) 0.0225(5) Uani 0.48(3) 2 d S T P
N3 N 0.0177(3) 0.57434(15) 0.37888(16) 0.0098(3) Uani 1 1 d . . .
N4 N 0.5186(3) 0.07479(15) 0.37899(16) 0.0100(3) Uani 1 1 d . . .
N5 N 0.0718(3) 0.09399(16) 0.17310(17) 0.0119(3) Uani 1 1 d . . .
H5 H 0.02(2) 0.029(15) 0.129(15) 0.11(3) Uiso 0.5 1 d . . P
N6 N 0.5837(3) 0.59393(16) 0.17146(17) 0.0126(3) Uani 1 1 d . . .
H6 H 0.60(2) 0.517(17) 0.126(14) 0.11(3) Uiso 0.5 1 d . . P
N7 N 0.0518(4) 0.2500 0.3889(2) 0.0093(3) Uani 1 2 d S T P
N8 N 0.4556(4) 0.2500 0.6163(2) 0.0094(4) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N -0.0010 0.0006
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and NIST'
Al Al 0.0100 0.0107
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and NIST'
P P 0.0200 0.0200
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and NIST'
O O 0.0000 0.0015
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and NIST'
H H 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and NIST'
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
N5 P1 N3 108.36(8) . 4_565
N5 P1 N7 108.18(9) . .
N3 P1 N7 110.86(8) 4_565 .
N5 P1 N4 112.25(7) . .
N3 P1 N4 109.02(7) 4_565 .
N7 P1 N4 108.19(8) . .
N6 P2 N4 109.92(8) 2_646 3_656
N6 P2 N8 107.25(9) 2_646 .
N4 P2 N8 110.85(8) 3_656 .
N6 P2 N3 110.59(8) 2_646 2_546
N4 P2 N3 108.75(7) 3_656 2_546
N8 P2 N3 109.49(8) . 2_546
O2 P3 N2 0.0 1_454 1_454
O2 P3 O1 107.30(12) 1_454 .
N2 P3 O1 107.30(12) 1_454 .
O2 P3 N5 112.61(7) 1_454 .
N2 P3 N5 112.61(7) 1_454 .
O1 P3 N5 109.60(7) . .
O2 P3 N5 112.61(7) 1_454 4_565
N2 P3 N5 112.61(7) 1_454 4_565
O1 P3 N5 109.59(7) . 4_565
N5 P3 N5 105.12(12) . 4_565
N1 P4 O1 0.0 1_556 1_556
N1 P4 N2 107.72(12) 1_556 .
O1 P4 N2 107.72(12) 1_556 .
N1 P4 N6 112.19(7) 1_556 2_646
O1 P4 N6 112.19(7) 1_556 2_646
N2 P4 N6 109.93(7) . 2_646
N1 P4 N6 112.19(7) 1_556 3_666
O1 P4 N6 112.19(7) 1_556 3_666
N2 P4 N6 109.93(8) . 3_666
N6 P4 N6 104.88(12) 2_646 3_666
N7 Al5 N8 178.66(9) 1_655 .
N7 Al5 N3 90.73(6) 1_655 3_666
N8 Al5 N3 88.31(6) . 3_666
N7 Al5 N3 90.73(6) 1_655 2_646
N8 Al5 N3 88.31(6) . 2_646
N3 Al5 N3 88.03(8) 3_666 2_646
N7 Al5 N4 89.29(6) 1_655 4_565
N8 Al5 N4 91.68(6) . 4_565
N3 Al5 N4 92.17(6) 3_666 4_565
N3 Al5 N4 179.80(6) 2_646 4_565
N7 Al5 N4 89.29(6) 1_655 .
N8 Al5 N4 91.68(6) . .
N3 Al5 N4 179.80(6) 3_666 .
N3 Al5 N4 92.17(6) 2_646 .
N4 Al5 N4 87.63(8) 4_565 .
P4 O1 P3 131.99(16) 1_554 .
P3 N2 P4 131.58(15) 1_656 .
P1 N3 P2 114.20(8) 4_565 2_556
P1 N3 Al5 123.67(8) 4_565 3_666
P2 N3 Al5 122.12(7) 2_556 3_666
P2 N4 P1 114.23(8) 3_656 .
P2 N4 Al5 123.69(8) 3_656 .
P1 N4 Al5 122.06(7) . .
P1 N5 P3 125.72(10) . .
P1 N5 H5 128(10) . .
P3 N5 H5 106(10) . .
P2 N6 P4 127.51(10) 2_656 3_666
P2 N6 H6 122(10) 2_656 .
P4 N6 H6 110(10) 3_666 .
P1 N7 P1 112.69(12) . 4_565
P1 N7 Al5 123.28(5) . 1_455
P1 N7 Al5 123.28(5) 4_565 1_455
P2 N8 P2 113.39(11) . 4_565
P2 N8 Al5 123.24(6) . .
P2 N8 Al5 123.24(6) 4_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 N5 1.6315(18) .
P1 N3 1.6413(14) 4_565
P1 N7 1.6454(11) .
P1 N4 1.6585(15) .
P2 N6 1.6373(18) 2_646
P2 N4 1.6426(14) 3_656
P2 N8 1.6453(11) .
P2 N3 1.6535(15) 2_546
P3 O2 1.603(3) 1_454
P3 N2 1.603(3) 1_454
P3 O1 1.6273(19) .
P3 N5 1.6361(15) .
P3 N5 1.6361(16) 4_565
P4 N1 1.602(2) 1_556
P4 O1 1.602(2) 1_556
P4 N2 1.616(2) .
P4 N6 1.6394(16) 2_646
P4 N6 1.6394(16) 3_666
Al5 N7 2.033(2) 1_655
Al5 N8 2.047(2) .
Al5 N3 2.1050(15) 3_666
Al5 N3 2.1050(15) 2_646
Al5 N4 2.1071(15) 4_565
Al5 N4 2.1072(15) .
O1 P4 1.602(2) 1_554
N2 P3 1.603(3) 1_656
N3 P1 1.6413(14) 4_565
N3 P2 1.6536(15) 2_556
N3 Al5 2.1050(15) 3_666
N4 P2 1.6426(14) 3_656
N5 H5 0.73(14) .
N6 P2 1.6373(18) 2_656
N6 P4 1.6393(16) 3_666
N6 H6 0.81(15) .
N7 P1 1.6455(11) 4_565
N7 Al5 2.033(2) 1_455
N8 P2 1.6453(11) 4_565
