#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/36/4513636.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_4513636
loop_
_publ_author_name
'Fu, Ruibiao'
'Hu, Shengmin'
'Wu, Xintao'
_publ_section_title
;
 Two New Zinc Phosphonates with Triazine-Based Phosphonic Acids
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5021
_journal_paper_doi               10.1021/acs.cgd.5b00983
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C17 H36 N3 O19.5 P3 Zn3'
_chemical_formula_weight         883.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.899(12)
_cell_angle_beta                 89.523(9)
_cell_angle_gamma                88.343(11)
_cell_formula_units_Z            2
_cell_length_a                   10.137(6)
_cell_length_b                   11.802(7)
_cell_length_c                   13.768(8)
_cell_measurement_reflns_used    3708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4719
_cell_measurement_theta_min      3.0314
_cell_volume                     1644.0(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       '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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12788
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.0800
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.223
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0838P)²+14.6176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2276
_reflns_number_gt                5003
_reflns_number_total             7027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00983_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513636--4513637.cif.
;
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C17 H36 N3 O19.50 P3 Zn3'
_cod_database_code               4513636
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Zn1 Zn 0.15736(8) 0.51598(8) 0.39554(6) 0.0224(2) Uani 1 1 d .
Zn2 Zn 0.55467(9) 0.57495(9) 0.37833(7) 0.0305(3) Uani 1 1 d .
Zn3 Zn 0.62257(11) 0.11009(10) -0.11254(9) 0.0417(3) Uani 1 1 d .
P1 P 0.3750(2) 0.3440(2) 0.42563(17) 0.0296(5) Uani 1 1 d .
P2 P 0.6707(2) 0.3352(2) -0.22994(15) 0.0269(5) Uani 1 1 d .
P3 P 0.84407(18) 0.46155(19) 0.37929(15) 0.0236(4) Uani 1 1 d .
O1 O 0.2294(5) 0.3604(5) 0.4049(4) 0.0308(13) Uani 1 1 d .
O2 O 0.4443(8) 0.4517(7) 0.3927(8) 0.073(3) Uani 1 1 d .
O3 O 0.4009(8) 0.3070(7) 0.5301(5) 0.056(2) Uani 1 1 d .
O4 O 0.4079(8) 0.0364(6) 0.1730(6) 0.057(2) Uani 1 1 d .
O5 O 0.1931(10) 0.0418(8) 0.1759(12) 0.122(5) Uani 1 1 d .
O6 O 0.7821(6) 0.3901(6) -0.2846(4) 0.0366(15) Uani 1 1 d .
O7 O 0.7159(7) 0.2158(6) -0.1897(5) 0.0465(18) Uani 1 1 d .
O8 O 0.5448(6) 0.3249(6) -0.2845(5) 0.0438(17) Uani 1 1 d .
O9 O 0.4405(7) 0.1451(6) -0.0850(6) 0.054(2) Uani 1 1 d .
O10 O 0.2432(7) 0.2162(7) -0.0545(7) 0.063(2) Uani 1 1 d .
O11 O 0.7301(5) 0.5343(6) 0.3370(5) 0.0356(14) Uani 1 1 d .
O12 O 0.9679(5) 0.5315(5) 0.3721(5) 0.0326(14) Uani 1 1 d .
O13 O 0.8182(6) 0.4131(5) 0.4816(4) 0.0328(14) Uani 1 1 d .
O14 O 1.1033(7) 0.3673(7) 0.0267(5) 0.053(2) Uani 1 1 d .
H1 H 1.1462 0.3164 0.0018 0.079 Uiso 1 1 calc R
O15 O 0.9855(8) 0.2250(7) 0.0847(7) 0.068(3) Uani 1 1 d .
O16 O 0.6846(19) 0.0682(12) 0.0212(10) 0.151(7) Uani 1 1 d .
O17 O 0.689(3) 0.202(2) 0.526(2) 0.263(13) Uani 1 1 d .
O18 O 1.0000 0.0000 0.0000 0.238(18) Uani 1 2 d S
O19 O 0.492(3) 0.0972(18) 0.6443(19) 0.280(17) Uani 1 1 d .
O20 O 0.095(3) -0.0800(12) 0.7591(17) 0.247(14) Uani 1 1 d .
N1 N 0.4166(7) 0.2462(6) 0.2528(5) 0.0290(15) Uani 1 1 d .
N2 N 0.8394(7) 0.3630(7) 0.2032(5) 0.0308(16) Uani 1 1 d .
N3 N 0.5516(7) 0.3591(7) -0.0547(5) 0.0342(17) Uani 1 1 d .
N4 N 0.4835(7) 0.2998(7) 0.0982(5) 0.0327(17) Uani 1 1 d .
N5 N 0.6297(7) 0.3031(6) 0.2310(5) 0.0293(15) Uani 1 1 d .
N6 N 0.7014(7) 0.3646(6) 0.0710(5) 0.0288(15) Uani 1 1 d .
N7 N -0.0455(15) 0.1339(15) 0.732(2) 0.200(14) Uani 1 1 d .
H2 H -0.1228 0.1355 0.7644 0.240 Uiso 1 1 calc R
H3 H -0.0105 0.0632 0.7415 0.240 Uiso 1 1 calc R
N8 N 0.1453(15) 0.2377(14) 0.6220(13) 0.113(5) Uani 1 1 d .
H4 H 0.1324 0.3130 0.6106 0.136 Uiso 1 1 calc R
H5 H 0.2226 0.2199 0.5932 0.136 Uiso 1 1 calc R
C1 C 0.5143(8) 0.2831(8) 0.1930(6) 0.0275(18) Uani 1 1 d .
C2 C 0.5811(9) 0.3421(8) 0.0419(6) 0.0305(19) Uani 1 1 d .
C3 C 0.7191(8) 0.3432(7) 0.1675(6) 0.0278(18) Uani 1 1 d .
C4 C 0.4394(8) 0.2275(7) 0.3576(6) 0.0275(18) Uani 1 1 d .
H4A H 0.5334 0.2180 0.3691 0.033 Uiso 1 1 calc R
H4B H 0.3976 0.1581 0.3808 0.033 Uiso 1 1 calc R
C5 C 0.2941(8) 0.2068(8) 0.2148(7) 0.0323(19) Uani 1 1 d .
H5A H 0.2694 0.2555 0.1585 0.039 Uiso 1 1 calc R
H5B H 0.2256 0.2153 0.2637 0.039 Uiso 1 1 calc R
C6 C 0.2978(11) 0.0853(10) 0.1856(9) 0.052(3) Uani 1 1 d .
C7 C 0.6405(9) 0.4165(8) -0.1242(7) 0.035(2) Uani 1 1 d .
H7C H 0.7237 0.4288 -0.0927 0.041 Uiso 1 1 calc R
H7D H 0.6021 0.4901 -0.1446 0.041 Uiso 1 1 calc R
C8 C 0.4122(8) 0.3486(9) -0.0812(6) 0.035(2) Uani 1 1 d .
H8C H 0.4004 0.3775 -0.1479 0.042 Uiso 1 1 calc R
H8D H 0.3581 0.3957 -0.0401 0.042 Uiso 1 1 calc R
C9 C 0.3637(9) 0.2293(9) -0.0716(7) 0.040(2) Uani 1 1 d .
C10 C 0.8688(8) 0.3403(8) 0.3061(6) 0.0294(18) Uani 1 1 d .
H10A H 0.9599 0.3136 0.3121 0.035 Uiso 1 1 calc R
H10B H 0.8134 0.2798 0.3316 0.035 Uiso 1 1 calc R
C11 C 0.9416(8) 0.4132(8) 0.1400(6) 0.034(2) Uani 1 1 d .
H11A H 1.0055 0.4493 0.1793 0.041 Uiso 1 1 calc R
H11B H 0.9017 0.4710 0.0959 0.041 Uiso 1 1 calc R
C12 C 1.0112(9) 0.3234(9) 0.0817(7) 0.038(2) Uani 1 1 d .
C13 C 0.0422(16) 0.2110(19) 0.7781(14) 0.106(6) Uani 1 1 d .
H13A H 0.0585 0.1832 0.8446 0.127 Uiso 1 1 calc R
H13B H -0.0008 0.2854 0.7799 0.127 Uiso 1 1 calc R
C14 C 0.1684(18) 0.2212(18) 0.7259(16) 0.115(7) Uani 1 1 d .
H14A H 0.2154 0.2850 0.7486 0.138 Uiso 1 1 calc R
H14B H 0.2224 0.1530 0.7389 0.138 Uiso 1 1 calc R
C15 C -0.077(5) 0.152(5) 0.623(3) 0.43(5) Uani 1 1 d .
H15A H -0.1073 0.0817 0.5977 0.522 Uiso 1 1 calc R
H15B H -0.1457 0.2098 0.6125 0.522 Uiso 1 1 calc R
C16 C 0.0505(18) 0.188(2) 0.569(2) 0.148(10) Uani 1 1 d .
H16A H 0.0912 0.1132 0.5856 0.178 Uiso 1 1 calc R
C17 C -0.004(11) 0.143(4) 0.471(3) 0.83(13) Uani 1 1 d .
H17A H 0.0606 0.1540 0.4201 1.249 Uiso 1 1 calc R
H17B H -0.0840 0.1846 0.4528 1.249 Uiso 1 1 calc R
H17C H -0.0221 0.0638 0.4799 1.249 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'
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'
Zn Zn 0.2839 1.4301 '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
O6 Zn1 O13 112.4(3) 2_665 2_666
O6 Zn1 O12 98.4(3) 2_665 1_455
O13 Zn1 O12 104.3(3) 2_666 1_455
O6 Zn1 O1 115.6(3) 2_665 .
O13 Zn1 O1 109.7(3) 2_666 .
O12 Zn1 O1 115.5(3) 1_455 .
O2 Zn2 O11 113.4(3) . .
O2 Zn2 O8 101.3(4) . 2_665
O11 Zn2 O8 114.5(3) . 2_665
O2 Zn2 O3 131.2(4) . 2_666
O11 Zn2 O3 98.7(3) . 2_666
O8 Zn2 O3 97.2(3) 2_665 2_666
O7 Zn3 O9 117.7(3) . .
O7 Zn3 O16 119.2(6) . .
O9 Zn3 O16 99.5(6) . .
O7 Zn3 O4 115.2(3) . 2_655
O9 Zn3 O4 96.2(3) . 2_655
O16 Zn3 O4 105.5(5) . 2_655
O3 P1 O1 112.2(4) . .
O3 P1 O2 113.4(6) . .
O1 P1 O2 108.7(4) . .
O3 P1 C4 104.3(4) . .
O1 P1 C4 108.8(4) . .
O2 P1 C4 109.3(4) . .
O6 P2 O8 116.6(4) . .
O6 P2 O7 109.5(4) . .
O8 P2 O7 108.6(4) . .
O6 P2 C7 106.5(4) . .
O8 P2 C7 109.8(4) . .
O7 P2 C7 105.3(4) . .
O13 P3 O11 113.7(4) . .
O13 P3 O12 112.6(4) . .
O11 P3 O12 108.0(4) . .
O13 P3 C10 105.6(4) . .
O11 P3 C10 108.5(4) . .
O12 P3 C10 108.3(4) . .
P1 O1 Zn1 117.4(4) . .
P1 O2 Zn2 166.1(8) . .
P1 O3 Zn2 118.2(5) . 2_666
C6 O4 Zn3 108.2(8) . 2_655
P2 O6 Zn1 149.0(4) . 2_665
P2 O7 Zn3 129.1(4) . .
P2 O8 Zn2 134.2(4) . 2_665
C9 O9 Zn3 140.5(7) . .
P3 O11 Zn2 135.7(4) . .
P3 O12 Zn1 140.3(4) . 1_655
P3 O13 Zn1 128.6(4) . 2_666
C1 N1 C5 121.3(7) . .
C1 N1 C4 120.5(7) . .
C5 N1 C4 117.4(7) . .
C3 N2 C10 121.1(7) . .
C3 N2 C11 120.4(7) . .
C10 N2 C11 118.4(7) . .
C2 N3 C7 122.5(7) . .
C2 N3 C8 116.4(7) . .
C7 N3 C8 118.8(7) . .
C2 N4 C1 114.5(7) . .
C1 N5 C3 114.7(7) . .
C2 N6 C3 113.1(7) . .
C13 N7 C15 120(3) . .
C16 N8 C14 126.8(17) . .
N5 C1 N4 125.2(7) . .
N5 C1 N1 118.5(7) . .
N4 C1 N1 116.3(7) . .
N6 C2 N4 126.1(8) . .
N6 C2 N3 118.6(7) . .
N4 C2 N3 115.3(8) . .
N5 C3 N2 116.6(8) . .
N5 C3 N6 126.3(8) . .
N2 C3 N6 117.1(7) . .
N1 C4 P1 112.2(6) . .
N1 C5 C6 115.3(8) . .
O5 C6 O4 124.4(13) . .
O5 C6 C5 116.8(11) . .
O4 C6 C5 118.8(10) . .
N3 C7 P2 111.9(6) . .
N3 C8 C9 114.2(8) . .
O10 C9 O9 120.9(9) . .
O10 C9 C8 117.8(9) . .
O9 C9 C8 121.2(8) . .
N2 C10 P3 114.2(6) . .
N2 C11 C12 110.9(8) . .
O15 C12 O14 123.7(9) . .
O15 C12 C11 125.2(9) . .
O14 C12 C11 111.1(9) . .
N7 C13 C14 111.7(18) . .
N8 C14 C13 110.0(15) . .
C16 C15 N7 108(4) . .
N8 C16 C15 118(3) . .
N8 C16 C17 152(4) . .
C15 C16 C17 90(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O6 1.944(6) 2_665
Zn1 O13 1.948(6) 2_666
Zn1 O12 1.951(6) 1_455
Zn1 O1 1.954(6) .
Zn2 O2 1.862(8) .
Zn2 O11 1.918(6) .
Zn2 O8 1.967(7) 2_665
Zn2 O3 1.992(8) 2_666
Zn3 O7 1.868(7) .
Zn3 O9 1.919(7) .
Zn3 O16 1.983(12) .
Zn3 O4 1.992(8) 2_655
P1 O3 1.504(7) .
P1 O1 1.510(6) .
P1 O2 1.516(8) .
P1 C4 1.808(9) .
P2 O6 1.495(6) .
P2 O8 1.498(7) .
P2 O7 1.544(7) .
P2 C7 1.806(10) .
P3 O13 1.515(6) .
P3 O11 1.520(6) .
P3 O12 1.522(6) .
P3 C10 1.805(9) .
O3 Zn2 1.992(8) 2_666
O4 C6 1.257(13) .
O4 Zn3 1.992(8) 2_655
O5 C6 1.204(14) .
O6 Zn1 1.944(6) 2_665
O8 Zn2 1.967(7) 2_665
O9 C9 1.265(12) .
O10 C9 1.254(11) .
O12 Zn1 1.951(5) 1_655
O13 Zn1 1.948(6) 2_666
O14 C12 1.298(11) .
O15 C12 1.196(12) .
N1 C1 1.349(10) .
N1 C5 1.450(11) .
N1 C4 1.468(11) .
N2 C3 1.349(11) .
N2 C10 1.459(11) .
N2 C11 1.465(10) .
N3 C2 1.367(11) .
N3 C7 1.462(10) .
N3 C8 1.473(11) .
N4 C2 1.342(10) .
N4 C1 1.348(11) .
N5 C1 1.318(11) .
N5 C3 1.333(10) .
N6 C2 1.326(11) .
N6 C3 1.352(11) .
N7 C13 1.46(3) .
N7 C15 1.54(5) .
N8 C16 1.37(3) .
N8 C14 1.45(2) .
C5 C6 1.509(15) .
C8 C9 1.502(14) .
C11 C12 1.518(13) .
C13 C14 1.47(2) .
C15 C16 1.54(4) .
C16 C17 1.59(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
O14 H1 O10 0.82 1.73 2.547(11) 176.1 1_655
N7 H2 O7 0.90 1.98 2.809(16) 152.3 1_456
N7 H3 O20 0.90 1.98 2.87(3) 170.3 .
N8 H4 O12 0.90 2.10 2.930(19) 153.7 2_666
N8 H5 O3 0.90 2.25 2.989(17) 139.2 .
