#------------------------------------------------------------------------------
#$Date: 2019-11-28 16:24:14 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244102 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/82/7238267.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_7238267
loop_
_publ_author_name
'Chen, Shuo-ping'
'Zhang, Yu-qin'
'Hu, Le'
'He, Hong-zhen'
'Yuan, Liang-jie'
_publ_section_title
;
 Hydrogen-bonded assembly of aminophosphonic anions: different 1D, 2D and
 3D supramolecular architectures
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              3327
_journal_paper_doi               10.1039/c003756g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C5 H21 N3 O7 P2'
_chemical_formula_weight         297.19
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7719(6)
_cell_length_b                   11.5346(8)
_cell_length_c                   12.2848(9)
_cell_measurement_temperature    273(2)
_cell_volume                     1242.98(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7916
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.9146
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_coef       0.0125(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2324
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0212
_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)+(0.0416P)²+0.0942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                2278
_reflns_number_total             2324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c003756g.txt
_cod_data_source_block           81210x_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7238267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, 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
P1 P 0.14404(4) 0.54924(3) 0.23867(4) 0.01683(10) Uani 1 1 d .
P2 P 0.42154(4) 0.58515(3) 0.08984(3) 0.01826(10) Uani 1 1 d .
N1 N 0.30038(13) 0.75182(10) 0.22065(11) 0.0183(2) Uani 1 1 d .
H1A H 0.2776 0.7758 0.2876 0.028 Uiso 1 1 calc R
H1B H 0.2229 0.7672 0.1762 0.028 Uiso 1 1 calc R
H1C H 0.3835 0.7885 0.1973 0.028 Uiso 1 1 calc R
O2 O 0.03614(12) 0.60307(9) 0.15738(10) 0.0213(2) Uani 1 1 d .
O3 O 0.09124(13) 0.55516(11) 0.35532(11) 0.0280(3) Uani 1 1 d .
O1 O 0.18140(14) 0.42107(9) 0.20924(13) 0.0289(3) Uani 1 1 d D
O4 O 0.58943(11) 0.61028(10) 0.10186(12) 0.0256(3) Uani 1 1 d .
C1 C 0.32951(15) 0.62294(12) 0.22211(13) 0.0163(3) Uani 1 1 d .
C2 C 0.43448(18) 0.59429(14) 0.31842(16) 0.0247(3) Uani 1 1 d .
H2A H 0.5319 0.6304 0.3076 0.037 Uiso 1 1 calc R
H2B H 0.4475 0.5118 0.3234 0.037 Uiso 1 1 calc R
H2C H 0.3897 0.6227 0.3845 0.037 Uiso 1 1 calc R
O6 O 0.34680(13) 0.66082(11) 0.00537(11) 0.0286(3) Uani 1 1 d .
O5 O 0.38861(15) 0.45520(10) 0.07583(13) 0.0323(3) Uani 1 1 d .
N3 N 0.05754(16) 0.67801(13) 0.92211(13) 0.0263(3) Uani 1 1 d .
H3A H 0.0132 0.6091 0.9143 0.039 Uiso 1 1 calc R
H3B H -0.0077 0.7271 0.9530 0.039 Uiso 1 1 calc R
H3C H 0.1398 0.6708 0.9640 0.039 Uiso 1 1 calc R
C5 C 0.19647(18) 0.63430(14) 0.75245(15) 0.0252(3) Uani 1 1 d .
H5A H 0.1553 0.5575 0.7658 0.030 Uiso 1 1 calc R
H5B H 0.3005 0.6356 0.7793 0.030 Uiso 1 1 calc R
C6 C 0.1028(2) 0.72279(14) 0.81438(16) 0.0271(3) Uani 1 1 d .
H6A H 0.1620 0.7931 0.8236 0.032 Uiso 1 1 calc R
H6B H 0.0123 0.7419 0.7727 0.032 Uiso 1 1 calc R
N2 N 0.18977(15) 0.54746(11) 0.56906(12) 0.0230(3) Uani 1 1 d .
H2D H 0.2763 0.5084 0.5784 0.034 Uiso 1 1 calc R
H2E H 0.1767 0.5623 0.4986 0.034 Uiso 1 1 calc R
H2F H 0.1120 0.5052 0.5934 0.034 Uiso 1 1 calc R
O1W O 0.30796(18) 0.84999(14) 0.42592(14) 0.0459(4) Uani 1 1 d D
C4 C 0.1970(2) 0.65765(15) 0.63011(16) 0.0341(4) Uani 1 1 d .
H4A H 0.1103 0.7057 0.6111 0.041 Uiso 1 1 calc R
H4B H 0.2891 0.6993 0.6104 0.041 Uiso 1 1 calc R
H2W1 H 0.252(2) 0.8923(18) 0.4651(19) 0.050(8) Uiso 1 1 d D
H1 H 0.254(3) 0.426(2) 0.161(2) 0.066(9) Uiso 1 1 d D
H1W1 H 0.3888(19) 0.888(2) 0.417(3) 0.069(10) Uiso 1 1 d 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'
P P 0.1023 0.0942 '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
O3 P1 O2 114.68(7)
O3 P1 O1 109.17(8)
O2 P1 O1 111.66(7)
O3 P1 C1 110.76(7)
O2 P1 C1 106.87(6)
O1 P1 C1 103.06(7)
O6 P2 O4 112.40(7)
O6 P2 O5 113.98(8)
O4 P2 O5 112.47(7)
O6 P2 C1 106.03(7)
O4 P2 C1 107.00(7)
O5 P2 C1 104.13(7)
C1 N1 H1A 109.5
C1 N1 H1B 109.5
H1A N1 H1B 109.5
C1 N1 H1C 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
P1 O1 H1 104.1(19)
N1 C1 C2 108.84(12)
N1 C1 P1 107.80(9)
C2 C1 P1 110.14(10)
N1 C1 P2 107.05(9)
C2 C1 P2 111.18(10)
P1 C1 P2 111.69(7)
C1 C2 H2A 109.5
C1 C2 H2B 109.5
H2A C2 H2B 109.5
C1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C6 N3 H3A 109.5
C6 N3 H3B 109.5
H3A N3 H3B 109.5
C6 N3 H3C 109.5
H3A N3 H3C 109.5
H3B N3 H3C 109.5
C6 C5 C4 112.17(15)
C6 C5 H5A 109.2
C4 C5 H5A 109.2
C6 C5 H5B 109.2
C4 C5 H5B 109.2
H5A C5 H5B 107.9
N3 C6 C5 111.14(14)
N3 C6 H6A 109.4
C5 C6 H6A 109.4
N3 C6 H6B 109.4
C5 C6 H6B 109.4
H6A C6 H6B 108.0
C4 N2 H2D 109.5
C4 N2 H2E 109.5
H2D N2 H2E 109.5
C4 N2 H2F 109.5
H2D N2 H2F 109.5
H2E N2 H2F 109.5
H2W1 O1W H1W1 105.8(15)
N2 C4 C5 110.36(14)
N2 C4 H4A 109.6
C5 C4 H4A 109.6
N2 C4 H4B 109.6
C5 C4 H4B 109.6
H4A C4 H4B 108.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 O3 1.5076(14)
P1 O2 1.5095(12)
P1 O1 1.5569(12)
P1 C1 1.8469(14)
P2 O6 1.5061(13)
P2 O4 1.5082(10)
P2 O5 1.5361(11)
P2 C1 1.8660(16)
N1 C1 1.5085(17)
N1 H1A 0.8900
N1 H1B 0.8900
N1 H1C 0.8900
O1 H1 0.871(10)
C1 C2 1.535(2)
C2 H2A 0.9600
C2 H2B 0.9600
C2 H2C 0.9600
N3 C6 1.475(2)
N3 H3A 0.8900
N3 H3B 0.8900
N3 H3C 0.8900
C5 C6 1.515(2)
C5 C4 1.527(2)
C5 H5A 0.9700
C5 H5B 0.9700
C6 H6A 0.9700
C6 H6B 0.9700
N2 C4 1.477(2)
N2 H2D 0.8900
N2 H2E 0.8900
N2 H2F 0.8900
O1W H2W1 0.844(10)
O1W H1W1 0.840(10)
C4 H4A 0.9700
C4 H4B 0.9700
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
O1W H1W1 O3 0.840(10) 2.038(11) 2.850(2) 163(3) 3_565
O1 H1 O5 0.871(10) 1.614(11) 2.479(2) 172(3) .
O1W H2W1 O5 0.844(10) 1.973(11) 2.800(2) 166(2) 4
N2 H2F O2 0.89 1.97 2.8494(17) 171.3 2_565
N2 H2E O3 0.89 1.91 2.766(2) 159.4 .
N2 H2D O4 0.89 1.83 2.6877(17) 161.5 2_665
N3 H3C O6 0.89 1.89 2.7430(18) 160.1 1_556
N3 H3B O6 0.89 1.93 2.8141(19) 174.2 3_466
N3 H3A O3 0.89 2.23 3.1000(19) 167.2 2_565
N1 H1C O2 0.89 1.90 2.7718(16) 167.1 3_565
N1 H1B O2 0.89 2.51 2.9867(16) 113.8 .
N1 H1B O4 0.89 2.05 2.8433(17) 147.9 3_465
N1 H1A O1W 0.89 1.92 2.765(2) 157.6 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O3 P1 C1 N1 -77.43(11)
O2 P1 C1 N1 48.13(11)
O1 P1 C1 N1 165.92(10)
O3 P1 C1 C2 41.19(12)
O2 P1 C1 C2 166.75(10)
O1 P1 C1 C2 -75.46(12)
O3 P1 C1 P2 165.25(7)
O2 P1 C1 P2 -69.19(8)
O1 P1 C1 P2 48.60(10)
O6 P2 C1 N1 -36.98(10)
O4 P2 C1 N1 83.18(10)
O5 P2 C1 N1 -157.54(9)
O6 P2 C1 C2 -155.73(10)
O4 P2 C1 C2 -35.57(12)
O5 P2 C1 C2 83.71(11)
O6 P2 C1 P1 80.79(9)
O4 P2 C1 P1 -159.04(7)
O5 P2 C1 P1 -39.76(9)
C4 C5 C6 N3 159.60(15)
C6 C5 C4 N2 -141.56(15)
