#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320237.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_4320237
loop_
_publ_author_name
'Hui-Hua Song'
'Li-Min Zheng'
'Zheming Wang'
'Chun-Hua Yan'
Xin
_publ_section_title
;
 Zinc Diphosphonates Templated by Organic Amines: Syntheses and
 Characterizations of [NH3(CH2)2NH3]Zn(hedpH2)2.2H2O and
 [NH3(CH2)nNH3]Zn2(hedpH)2.2H2O (n= 4, 5, 6) (hedp =
 1-Hydroxyethylidenediphosphonate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5024
_journal_page_last               5029
_journal_paper_doi               10.1021/ic010033v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C6 H26 N2 O16 P4 Zn'
_chemical_formula_weight         571.54
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 117.790(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.7422(15)
_cell_length_b                   5.2889(2)
_cell_length_c                   16.0338(10)
_cell_measurement_reflns_used    17793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      3.48
_cell_volume                     1856.17(18)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Denzo & maXus'
_computing_molecular_graphics    'Bruker SHELXTL (1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.73
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17793
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing (1995, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2710
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0518P)²+3.4713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                2083
_reflns_number_total             2710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010033v_1.cif
_cod_data_source_block           '[NH3(CH2)2NH3]Zn(hedpH2)2.2H2O_(znen)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320237
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.0000 0.5000 0.0000 0.01614(14) Uani 1 2 d S . .
P1 P 0.06261(3) 0.99354(11) 0.14803(4) 0.01444(16) Uani 1 1 d . . .
P2 P 0.12469(3) 0.79483(12) 0.03397(5) 0.01590(16) Uani 1 1 d . . .
O1 O 0.01078(8) 0.8168(3) 0.08939(13) 0.0195(4) Uani 1 1 d . . .
O2 O 0.05612(8) 1.2660(3) 0.11923(13) 0.0205(4) Uani 1 1 d . . .
O3 O 0.07517(10) 0.9919(3) 0.25390(14) 0.0252(4) Uani 1 1 d . . .
H3 H 0.0705 0.8483 0.2687 0.038 Uiso 1 1 calc R . .
O4 O 0.07538(8) 0.5980(4) -0.01156(13) 0.0202(4) Uani 1 1 d . . .
O5 O 0.18603(8) 0.7248(4) 0.04274(14) 0.0231(4) Uani 1 1 d . . .
O6 O 0.10582(9) 1.0511(3) -0.02115(15) 0.0229(4) Uani 1 1 d . . .
H6 H 0.1187 1.1690 0.0163 0.034 Uiso 1 1 calc R . .
O7 O 0.14558(8) 0.6226(3) 0.20334(13) 0.0220(4) Uani 1 1 d . . .
H7 H 0.1183 0.5210 0.1735 0.033 Uiso 1 1 calc R . .
O1W O 0.07235(13) 0.5358(4) 0.31879(18) 0.0410(6) Uani 1 1 d D . .
H1WB H 0.072(2) 0.512(7) 0.3762(19) 0.061 Uiso 1 1 d D . .
H1WA H 0.0599(19) 0.383(5) 0.285(2) 0.061 Uiso 1 1 d D . .
N1 N 0.20979(11) 0.5089(4) 0.40473(18) 0.0244(5) Uani 1 1 d . . .
H1C H 0.2424 0.4191 0.4133 0.037 Uiso 1 1 calc R . .
H1B H 0.1848 0.5251 0.3433 0.037 Uiso 1 1 calc R . .
H1A H 0.1903 0.4301 0.4319 0.037 Uiso 1 1 calc R . .
C1 C 0.13271(11) 0.8599(5) 0.15231(18) 0.0171(5) Uani 1 1 d . . .
C2 C 0.18707(12) 1.0322(5) 0.2070(2) 0.0238(6) Uani 1 1 d . . .
H2C H 0.1892 1.0735 0.2667 0.036 Uiso 1 1 calc R . .
H2B H 0.1825 1.1845 0.1717 0.036 Uiso 1 1 calc R . .
H2A H 0.2239 0.9475 0.2171 0.036 Uiso 1 1 calc R . .
C3 C 0.22946(13) 0.7628(5) 0.4475(2) 0.0252(6) Uani 1 1 d . . .
H3B H 0.1939 0.8635 0.4362 0.030 Uiso 1 1 calc R . .
H3A H 0.2513 0.8482 0.4187 0.030 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
_geom_angle_publ_flag
O4 Zn1 O4 180.00(9) 5_565 . ?
O4 Zn1 O1 88.37(7) 5_565 . ?
O4 Zn1 O1 91.63(7) . . ?
O4 Zn1 O1 91.63(7) 5_565 5_565 ?
O4 Zn1 O1 88.37(7) . 5_565 ?
O1 Zn1 O1 180.00(9) . 5_565 ?
O4 Zn1 O2 90.67(7) 5_565 1_545 ?
O4 Zn1 O2 89.33(7) . 1_545 ?
O1 Zn1 O2 91.60(7) . 1_545 ?
O1 Zn1 O2 88.40(7) 5_565 1_545 ?
O4 Zn1 O2 89.33(7) 5_565 5_575 ?
O4 Zn1 O2 90.67(7) . 5_575 ?
O1 Zn1 O2 88.40(7) . 5_575 ?
O1 Zn1 O2 91.60(7) 5_565 5_575 ?
O2 Zn1 O2 180.00(7) 1_545 5_575 ?
O2 P1 O1 117.75(10) . . ?
O2 P1 O3 106.02(10) . . ?
O1 P1 O3 110.55(11) . . ?
O2 P1 C1 110.11(11) . . ?
O1 P1 C1 107.27(11) . . ?
O3 P1 C1 104.35(12) . . ?
O5 P2 O4 115.38(11) . . ?
O5 P2 O6 106.76(11) . . ?
O4 P2 O6 111.31(11) . . ?
O5 P2 C1 109.24(11) . . ?
O4 P2 C1 107.54(11) . . ?
O6 P2 C1 106.25(11) . . ?
P1 O1 Zn1 134.97(11) . . ?
P1 O2 Zn1 139.29(11) . 1_565 ?
P1 O3 H3 109.5 . . ?
P2 O4 Zn1 134.73(11) . . ?
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
H1WB O1W H1WA 107(2) . . ?
C3 N1 H1C 109.5 . . ?
C3 N1 H1B 109.5 . . ?
H1C N1 H1B 109.5 . . ?
C3 N1 H1A 109.5 . . ?
H1C N1 H1A 109.5 . . ?
H1B N1 H1A 109.5 . . ?
O7 C1 C2 106.9(2) . . ?
O7 C1 P1 107.94(17) . . ?
C2 C1 P1 110.83(18) . . ?
O7 C1 P2 107.99(16) . . ?
C2 C1 P2 110.30(19) . . ?
P1 C1 P2 112.62(13) . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2C C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
H2C C2 H2A 109.5 . . ?
H2B C2 H2A 109.5 . . ?
N1 C3 C3 109.8(3) . 7_566 ?
N1 C3 H3B 109.7 . . ?
C3 C3 H3B 109.7 7_566 . ?
N1 C3 H3A 109.7 . . ?
C3 C3 H3A 109.7 7_566 . ?
H3B C3 H3A 108.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 2.0259(18) 5_565 ?
Zn1 O4 2.0259(18) . ?
Zn1 O1 2.1393(18) . ?
Zn1 O1 2.1393(18) 5_565 ?
Zn1 O2 2.1538(18) 1_545 ?
Zn1 O2 2.1538(18) 5_575 ?
P1 O2 1.4988(18) . ?
P1 O1 1.5093(18) . ?
P1 O3 1.577(2) . ?
P1 C1 1.845(3) . ?
P2 O5 1.5040(19) . ?
P2 O4 1.5080(18) . ?
P2 O6 1.5655(19) . ?
P2 C1 1.846(3) . ?
O2 Zn1 2.1538(18) 1_565 ?
O3 H3 0.8200 . ?
O6 H6 0.8200 . ?
O7 C1 1.450(3) . ?
O7 H7 0.8200 . ?
O1W H1WB 0.935(18) . ?
O1W H1WA 0.940(18) . ?
N1 C3 1.483(3) . ?
N1 H1C 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1A 0.8900 . ?
C1 C2 1.519(3) . ?
C2 H2C 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2A 0.9600 . ?
C3 C3 1.514(6) 7_566 ?
C3 H3B 0.9700 . ?
C3 H3A 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
O3 H3 O1W 0.82 1.83 2.641(3) 170.6 .
O6 H6 O4 0.82 2.46 3.011(3) 125.6 1_565
O7 H7 O2 0.82 1.92 2.737(3) 172.5 1_545
N1 H1C O5 0.89 1.88 2.754(3) 168.1 4_545
N1 H1B O7 0.89 2.05 2.920(3) 164.8 .
N1 H1A O5 0.89 2.00 2.825(3) 153.0 6_566
O1W H1WB O4 0.935(18) 1.85(2) 2.778(3) 169(3) 6_566
O1W H1WA O3 0.940(18) 2.20(3) 3.071(3) 153(4) 1_545
