#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:50:20 +0300 (Fri, 06 May 2016) $
#$Revision: 182737 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/87/7038763.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_7038763
loop_
_publ_author_name
'Hou, Xiaomin'
'Tang, Si-Fu'
_publ_section_title
;
 Speciation of metal phosphonates with the assistance of weak
 interactions.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7349
_journal_page_last               7359
_journal_paper_doi               10.1039/c6dt00643d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C17 H16 N2 O6 P2 Zn'
_chemical_formula_weight         471.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-09 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                93.404(2)
_cell_angle_beta                 107.127(2)
_cell_angle_gamma                102.703(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6253(11)
_cell_length_b                   9.2656(12)
_cell_length_c                   12.1600(15)
_cell_measurement_reflns_used    8538
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.27
_cell_volume                     897.9(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8534
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.273
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0380
_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)+(0.0353P)²+0.3536P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3117
_reflns_number_total             4013
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt00643d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7038759--7038764.cif.'
_cod_database_code               7038763
_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.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.67646(4) 0.64169(4) 0.88564(3) 0.02060(11) Uani 1 1 d . .
O1 O 0.6651(3) 0.6169(2) 0.61947(18) 0.0281(5) Uani 1 1 d . .
O2 O 0.5087(2) 0.3441(2) 0.57675(18) 0.0274(5) Uani 1 1 d . .
H2B H 0.4727 0.3749 0.5148 0.041 Uiso 1 1 calc R U
O3 O 0.6719(2) 0.4628(2) 0.78222(17) 0.0239(5) Uani 1 1 d . .
O4 O 1.4237(2) 0.5743(2) 0.86120(18) 0.0249(5) Uani 1 1 d . .
O5 O 1.4069(3) 0.2985(2) 0.83477(19) 0.0290(5) Uani 1 1 d . .
H5A H 1.4870 0.3356 0.8136 0.043 Uiso 1 1 calc R U
O6 O 1.2465(3) 0.3915(3) 0.95289(18) 0.0320(5) Uani 1 1 d . .
N1 N 0.6482(3) 0.8339(3) 0.8100(2) 0.0229(6) Uani 1 1 d . .
N2 N 0.9357(3) 0.7654(3) 0.9078(2) 0.0254(6) Uani 1 1 d . .
P1 P 0.66068(9) 0.45971(9) 0.65456(7) 0.02037(18) Uani 1 1 d . .
P2 P 1.31270(9) 0.42213(9) 0.85341(7) 0.02022(18) Uani 1 1 d . .
C1 C 0.4987(4) 0.8579(4) 0.7584(3) 0.0335(8) Uani 1 1 d . .
H1A H 0.4048 0.7982 0.7702 0.040 Uiso 1 1 calc R U
C2 C 0.4782(5) 0.9678(4) 0.6882(4) 0.0487(10) Uani 1 1 d . .
H2A H 0.3729 0.9848 0.6557 0.058 Uiso 1 1 calc R U
C3 C 0.6148(5) 1.0515(4) 0.6668(4) 0.0484(11) Uani 1 1 d . .
H3A H 0.6028 1.1228 0.6163 0.058 Uiso 1 1 calc R U
C4 C 0.7709(4) 1.0296(4) 0.7207(3) 0.0373(8) Uani 1 1 d . .
H4A H 0.8656 1.0874 0.7085 0.045 Uiso 1 1 calc R U
C5 C 0.7845(4) 0.9206(3) 0.7931(3) 0.0247(7) Uani 1 1 d . .
C6 C 0.9473(4) 0.8908(3) 0.8570(3) 0.0219(6) Uani 1 1 d . .
C7 C 1.1004(4) 0.9860(4) 0.8672(3) 0.0332(8) Uani 1 1 d . .
H7A H 1.1058 1.0730 0.8326 0.040 Uiso 1 1 calc R U
C8 C 1.2449(4) 0.9495(4) 0.9296(3) 0.0390(9) Uani 1 1 d . .
H8A H 1.3491 1.0120 0.9377 0.047 Uiso 1 1 calc R U
C9 C 1.2341(4) 0.8210(4) 0.9794(3) 0.0390(9) Uani 1 1 d . .
H9A H 1.3303 0.7932 1.0199 0.047 Uiso 1 1 calc R U
C10 C 1.0771(4) 0.7330(4) 0.9684(3) 0.0330(8) Uani 1 1 d . .
H10A H 1.0698 0.6474 1.0049 0.040 Uiso 1 1 calc R U
C11 C 0.9750(4) 0.2100(4) 0.4117(3) 0.0403(9) Uani 1 1 d . .
H11A H 0.8668 0.1993 0.3557 0.060 Uiso 1 1 calc R U
H11B H 0.9943 0.1131 0.4235 0.060 Uiso 1 1 calc R U
H11C H 1.0598 0.2664 0.3839 0.060 Uiso 1 1 calc R U
C12 C 0.9813(4) 0.2902(3) 0.5248(3) 0.0252(7) Uani 1 1 d . .
C13 C 1.1232(4) 0.3178(3) 0.6212(3) 0.0259(7) Uani 1 1 d . .
H13A H 1.2172 0.2891 0.6145 0.031 Uiso 1 1 calc R U
C14 C 1.1296(3) 0.3869(3) 0.7275(2) 0.0196(6) Uani 1 1 d . .
C15 C 0.9880(4) 0.4302(3) 0.7364(2) 0.0216(6) Uani 1 1 d . .
H15A H 0.9898 0.4755 0.8073 0.026 Uiso 1 1 calc R U
C16 C 0.8442(3) 0.4065(3) 0.6408(2) 0.0198(6) Uani 1 1 d . .
C17 C 0.8432(4) 0.3371(3) 0.5357(3) 0.0248(7) Uani 1 1 d . .
H17A H 0.7480 0.3217 0.4712 0.030 Uiso 1 1 calc R U
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'
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'
N N 0.0061 0.0033 '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 O3 109.55(9) 2_767 .
O6 Zn1 O4 97.33(9) 2_767 1_455
O3 Zn1 O4 92.68(8) . 1_455
O6 Zn1 N1 131.75(10) 2_767 .
O3 Zn1 N1 117.36(9) . .
O4 Zn1 N1 91.34(9) 1_455 .
O6 Zn1 N2 87.70(9) 2_767 .
O3 Zn1 N2 97.25(9) . .
O4 Zn1 N2 166.69(9) 1_455 .
N1 Zn1 N2 76.24(10) . .
P1 O3 Zn1 125.08(12) . .
P2 O4 Zn1 130.76(12) . 1_655
P2 O6 Zn1 140.01(13) . 2_767
C1 N1 C5 118.8(3) . .
C1 N1 Zn1 122.5(2) . .
C5 N1 Zn1 117.3(2) . .
C10 N2 C6 118.2(3) . .
C10 N2 Zn1 127.6(2) . .
C6 N2 Zn1 114.1(2) . .
O2 P1 O3 112.08(12) . .
O2 P1 O1 112.14(12) . .
O3 P1 O1 109.64(12) . .
O2 P1 C16 107.44(13) . .
O3 P1 C16 106.73(12) . .
O1 P1 C16 108.58(13) . .
O6 P2 O4 116.97(13) . .
O6 P2 O5 108.55(13) . .
O4 P2 O5 109.76(12) . .
O6 P2 C14 104.91(12) . .
O4 P2 C14 110.67(13) . .
O5 P2 C14 105.26(13) . .
N1 C1 C2 122.4(3) . .
C3 C2 C1 118.9(3) . .
C2 C3 C4 119.4(3) . .
C3 C4 C5 119.0(3) . .
N1 C5 C4 121.3(3) . .
N1 C5 C6 115.7(3) . .
C4 C5 C6 123.0(3) . .
N2 C6 C7 121.9(3) . .
N2 C6 C5 115.0(3) . .
C7 C6 C5 123.1(3) . .
C8 C7 C6 118.8(3) . .
C9 C8 C7 119.6(3) . .
C8 C9 C10 118.6(3) . .
N2 C10 C9 122.8(3) . .
C13 C12 C17 118.2(3) . .
C13 C12 C11 121.1(3) . .
C17 C12 C11 120.7(3) . .
C12 C13 C14 122.0(3) . .
C13 C14 C15 118.5(3) . .
C13 C14 P2 122.4(2) . .
C15 C14 P2 119.1(2) . .
C16 C15 C14 121.0(3) . .
C15 C16 C17 118.7(3) . .
C15 C16 P1 120.4(2) . .
C17 C16 P1 120.8(2) . .
C12 C17 C16 121.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O6 1.945(2) 2_767
Zn1 O3 2.006(2) .
Zn1 O4 2.057(2) 1_455
Zn1 N1 2.081(2) .
Zn1 N2 2.206(3) .
O1 P1 1.537(2) .
O2 P1 1.514(2) .
O3 P1 1.525(2) .
O4 P2 1.500(2) .
O4 Zn1 2.057(2) 1_655
O5 P2 1.585(2) .
O6 P2 1.499(2) .
O6 Zn1 1.945(2) 2_767
N1 C1 1.331(4) .
N1 C5 1.348(4) .
N2 C10 1.334(4) .
N2 C6 1.346(4) .
P1 C16 1.807(3) .
P2 C14 1.798(3) .
C1 C2 1.376(5) .
C2 C3 1.363(5) .
C3 C4 1.378(5) .
C4 C5 1.381(4) .
C5 C6 1.485(4) .
C6 C7 1.384(4) .
C7 C8 1.380(5) .
C8 C9 1.365(5) .
C9 C10 1.382(4) .
C11 C12 1.505(4) .
C12 C13 1.386(4) .
C12 C17 1.392(4) .
C13 C14 1.389(4) .
C14 C15 1.397(4) .
C15 C16 1.393(4) .
C16 C17 1.393(4) .
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
O2 H2B O1 0.82 1.73 2.511(3) 158.3 2_666
O5 H5A O3 0.82 1.91 2.719(3) 167.1 1_655
C1 H1A O4 0.93 2.42 3.001(4) 120.3 1_455
C13 H13A O5 0.93 2.68 3.044(4) 104.1 .
C15 H15A O3 0.93 2.64 3.012(3) 104.4 .
C15 H15A O6 0.93 2.69 3.005(3) 100.5 .
C17 H17A O2 0.93 2.77 3.083(4) 100.9 .
