#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:05:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180411 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/80/7208019.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_7208019
loop_
_publ_author_name
'Yamada, Teppei'
'Kitagawa, Hiroshi'
_publ_section_title
;
 Syntheses of metal--organic frameworks with protected phosphonate ligands
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4148
_journal_paper_doi               10.1039/c2ce25358e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C16 H21 N O10 P Zn'
_chemical_formula_weight         483.72
_chemical_name_common
;
dizinc 4,4'-bipyridyl bis(3-etacarboxy-5-carboxylphoshonate trihydrate
;
_chemical_name_systematic
;
dizinc 4,4'-bipyridyl bis(3-etacarboxy-5-carboxylphoshonate trihydrate
;
_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                110.960(2)
_cell_angle_beta                 96.523(3)
_cell_angle_gamma                108.941(2)
_cell_formula_units_Z            2
_cell_length_a                   8.463(2)
_cell_length_b                   11.263(3)
_cell_length_c                   11.774(3)
_cell_measurement_reflns_used    ' 8242'
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      ' 27.63'
_cell_measurement_theta_min      ' 2.17'
_cell_volume                     957.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker APEX-II CCD-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8843
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.8708
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0262
_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)+(0.0409P)²+0.7965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                3269
_reflns_number_total             3348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25358e.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7208019
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
Zn1 Zn 0.64466(3) 0.03072(2) 0.30826(2) 0.01311(10) Uani 1 1 d
C1 C 0.2037(2) -0.0378(2) 0.18674(19) 0.0137(4) Uani 1 1 d
C2 C 0.2466(3) -0.0349(2) 0.07616(19) 0.0141(4) Uani 1 1 d
C3 C 0.2372(2) 0.0671(2) 0.03803(19) 0.0131(4) Uani 1 1 d
C4 C 0.1862(2) 0.1682(2) 0.11208(19) 0.0141(4) Uani 1 1 d
C5 C 0.1414(2) 0.1653(2) 0.22156(19) 0.0143(4) Uani 1 1 d
C6 C 0.1485(3) 0.0618(2) 0.25860(19) 0.0142(4) Uani 1 1 d
P1 P 0.23824(7) -0.16077(5) 0.24137(5) 0.01291(13) Uani 1 1 d
O1 O 0.43011(18) -0.11127(14) 0.29769(13) 0.0161(3) Uani 1 1 d
O2 O 0.12781(19) -0.18222(15) 0.32989(14) 0.0174(3) Uani 1 1 d
O3 O 0.17505(18) -0.30065(14) 0.11922(14) 0.0173(3) Uani 1 1 d
C7 C 0.2926(3) -0.3605(2) 0.0601(2) 0.0215(5) Uani 1 1 d
C8 C 0.2995(4) -0.4687(3) 0.1041(3) 0.0366(6) Uani 1 1 d
H8 H 0.279(3) -0.102(3) 0.026(2) 0.023(6) Uiso 1 1 d
H8A H 0.435(3) 0.351(3) 0.591(2) 0.018(6) Uiso 1 1 d
H8B H 0.121(3) 0.060(2) 0.329(2) 0.010(5) Uiso 1 1 d
H8C H 0.508(3) 0.166(3) 0.522(2) 0.024(6) Uiso 1 1 d
H8D H 0.402(3) -0.289(3) 0.089(2) 0.019(6) Uiso 1 1 d
H8E H 0.701(3) 0.285(3) 0.274(2) 0.020(6) Uiso 1 1 d
H8F H 0.640(4) 0.481(3) 0.344(3) 0.032(7) Uiso 1 1 d
H8G H 0.180(3) 0.236(3) 0.085(2) 0.025(7) Uiso 1 1 d
H8H H 0.804(4) -0.065(3) 0.407(3) 0.033(8) Uiso 1 1 d
C9 C 0.2195(4) -0.4194(3) -0.0802(2) 0.0336(6) Uani 1 1 d
H9 H 0.134(4) 0.239(3) 0.695(3) 0.036(9) Uiso 1 1 d
H9A H 0.828(3) 0.057(3) 0.497(3) 0.021(7) Uiso 1 1 d
H9B H 0.303(4) -0.455(3) -0.123(3) 0.047(9) Uiso 1 1 d
H9C H 0.069(4) 0.652(4) 0.367(3) 0.042(8) Uiso 1 1 d
H9D H 0.377(4) -0.510(3) 0.067(3) 0.043(8) Uiso 1 1 d
H9E H 0.101(5) -0.505(4) -0.110(3) 0.057(10) Uiso 1 1 d
H9F H 0.005(4) 0.613(3) 0.448(3) 0.041(9) Uiso 1 1 d
H9G H 0.203(4) -0.347(4) -0.107(3) 0.052(9) Uiso 1 1 d
H9H H 0.252(5) 0.230(4) 0.765(4) 0.056(10) Uiso 1 1 d
C10 C 0.2791(2) 0.0690(2) -0.08225(19) 0.0148(4) Uani 1 1 d
H9I H 0.079(5) 0.442(5) 0.319(4) 0.080(13) Uiso 1 1 d
H10 H 0.341(5) -0.429(4) 0.195(4) 0.058(10) Uiso 1 1 d
H10A H 0.177(5) -0.551(4) 0.076(4) 0.065(11) Uiso 1 1 d
O4 O 0.30284(19) -0.03737(15) -0.15396(13) 0.0177(3) Uani 1 1 d
O5 O 0.2890(2) 0.16871(16) -0.10722(14) 0.0197(3) Uani 1 1 d
C11 C 0.0882(3) 0.2743(2) 0.3033(2) 0.0168(4) Uani 1 1 d
O6 O 0.0498(2) 0.27665(17) 0.39971(16) 0.0287(4) Uani 1 1 d
O7 O 0.0921(2) 0.36796(18) 0.26033(16) 0.0288(4) Uani 1 1 d
N1 N 0.6074(2) 0.20762(17) 0.38700(16) 0.0145(3) Uani 1 1 d
C12 C 0.5314(3) 0.2303(2) 0.4823(2) 0.0163(4) Uani 1 1 d
C13 C 0.4875(3) 0.3428(2) 0.5286(2) 0.0166(4) Uani 1 1 d
C14 C 0.5237(3) 0.4394(2) 0.47674(19) 0.0146(4) Uani 1 1 d
C15 C 0.6061(3) 0.4163(2) 0.3794(2) 0.0236(5) Uani 1 1 d
C16 C 0.6449(3) 0.3011(2) 0.3377(2) 0.0211(5) Uani 1 1 d
O8 O 0.8095(2) 0.01478(18) 0.42750(17) 0.0191(3) Uani 1 1 d
O9 O 0.2266(2) 0.24478(17) 0.69634(16) 0.0223(3) Uani 1 1 d
O10 O 0.0285(2) 0.57968(17) 0.38370(17) 0.0226(3) Uani 1 1 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'
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
O4 Zn1 O1 118.99(6) 2_655 .
O4 Zn1 O8 119.77(7) 2_655 .
O1 Zn1 O8 100.53(7) . .
O4 Zn1 N1 101.73(6) 2_655 .
O1 Zn1 N1 103.41(7) . .
O8 Zn1 N1 111.53(7) . .
C6 C1 C2 119.25(18) . .
C6 C1 P1 120.90(15) . .
C2 C1 P1 119.63(15) . .
C3 C2 C1 120.98(18) . .
C4 C3 C2 119.32(18) . .
C4 C3 C10 119.36(17) . .
C2 C3 C10 121.31(18) . .
C3 C4 C5 120.11(18) . .
C4 C5 C6 120.47(18) . .
C4 C5 C11 120.81(18) . .
C6 C5 C11 118.71(18) . .
C1 C6 C5 119.83(19) . .
O2 P1 O1 114.25(8) . .
O2 P1 O3 108.73(8) . .
O1 P1 O3 109.74(8) . .
O2 P1 C1 110.15(9) . .
O1 P1 C1 108.43(9) . .
O3 P1 C1 105.14(9) . .
P1 O1 Zn1 137.92(9) . .
C7 O3 P1 123.96(14) . .
O3 C7 C8 108.21(18) . .
O3 C7 C9 106.52(19) . .
C8 C7 C9 112.6(2) . .
O5 C10 O4 124.00(18) . .
O5 C10 C3 120.17(18) . .
O4 C10 C3 115.82(17) . .
C10 O4 Zn1 114.33(13) . 2_655
O6 C11 O7 124.13(19) . .
O6 C11 C5 123.06(19) . .
O7 C11 C5 112.79(18) . .
C12 N1 C16 117.90(17) . .
C12 N1 Zn1 121.52(13) . .
C16 N1 Zn1 120.34(14) . .
N1 C12 C13 122.67(19) . .
C12 C13 C14 119.83(19) . .
C13 C14 C15 117.02(19) . .
C13 C14 C14 121.2(2) . 2_666
C15 C14 C14 121.8(2) . 2_666
C16 C15 C14 119.8(2) . .
N1 C16 C15 122.76(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.9397(15) 2_655
Zn1 O1 1.9470(14) .
Zn1 O8 1.9615(16) .
Zn1 N1 2.0202(17) .
C1 C6 1.394(3) .
C1 C2 1.399(3) .
C1 P1 1.810(2) .
C2 C3 1.396(3) .
C3 C4 1.392(3) .
C3 C10 1.504(3) .
C4 C5 1.392(3) .
C5 C6 1.398(3) .
C5 C11 1.500(3) .
P1 O2 1.5076(14) .
P1 O1 1.5134(15) .
P1 O3 1.5792(15) .
O3 C7 1.479(3) .
C7 C8 1.499(3) .
C7 C9 1.507(4) .
C10 O5 1.239(3) .
C10 O4 1.288(3) .
O4 Zn1 1.9397(15) 2_655
C11 O6 1.210(3) .
C11 O7 1.316(3) .
N1 C12 1.343(3) .
N1 C16 1.345(3) .
C12 C13 1.377(3) .
C13 C14 1.397(3) .
C14 C15 1.398(3) .
C14 C14 1.482(4) 2_666
C15 C16 1.374(3) .
