#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320238.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_4320238
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            'C8 H28 N2 O16 P4 Zn2'
_chemical_formula_weight         662.94
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.619(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4970(3)
_cell_length_b                   12.1041(6)
_cell_length_c                   16.2814(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.31
_cell_measurement_theta_min      8.29
_cell_volume                     1071.07(11)
_computing_cell_refinement       'Enraf Nonius CAD4'
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        'Enraf Nonius MolEN 4.00'
_computing_molecular_graphics    'Siemens SHELXTL (1990)'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf Nonius CAD4 Mach3'
_diffrn_measurement_method       theta/2theta
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.028548
_diffrn_orient_matrix_UB_12      0.081167
_diffrn_orient_matrix_UB_13      -0.004938
_diffrn_orient_matrix_UB_21      0.018642
_diffrn_orient_matrix_UB_22      -0.009951
_diffrn_orient_matrix_UB_23      -0.059711
_diffrn_orient_matrix_UB_31      -0.180808
_diffrn_orient_matrix_UB_32      0.011767
_diffrn_orient_matrix_UB_33      -0.016410
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2832
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North,Philips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.0059(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0517P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                2200
_reflns_number_total             2573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010033v_2.cif
_cod_data_source_block           '[NH3(CH2)4NH3]Zn2(hedpH)2.2H2O_(znbn1)'
_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.

'_exptl_absorpt_correction_type' value 'psi scan'
changed to 'psi-scan' 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               4320238
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.29152(6) 0.56206(3) 0.421623(18) 0.01397(12) Uani 1 1 d . . .
P1 P 0.79283(12) 0.42101(5) 0.38210(4) 0.01029(16) Uani 1 1 d . . .
P2 P 0.74117(12) 0.66553(5) 0.35514(4) 0.01171(16) Uani 1 1 d . . .
O1 O 0.6510(4) 0.43739(16) 0.45382(12) 0.0162(4) Uani 1 1 d . . .
O1W O 0.2696(5) 0.3572(2) 0.1932(2) 0.0433(7) Uani 1 1 d . . .
H1WB H 0.141(9) 0.320(4) 0.195(3) 0.052 Uiso 1 1 d . . .
H1WA H 0.388(8) 0.302(4) 0.187(3) 0.052 Uiso 1 1 d . . .
O2 O 1.0685(4) 0.43041(15) 0.40059(13) 0.0165(4) Uani 1 1 d . . .
O3 O 0.7194(4) 0.30651(16) 0.34369(12) 0.0190(4) Uani 1 1 d . . .
H3 H 0.790(12) 0.287(6) 0.295(5) 0.13(3) Uiso 1 1 d . . .
O4 O 0.5703(3) 0.67465(15) 0.42013(11) 0.0146(4) Uani 1 1 d . . .
O5 O 1.0129(4) 0.67444(16) 0.38670(13) 0.0197(4) Uani 1 1 d . . .
O6 O 0.6588(4) 0.75222(17) 0.28786(13) 0.0217(5) Uani 1 1 d . . .
O7 O 0.4092(4) 0.52311(17) 0.29642(13) 0.0165(4) Uani 1 1 d . . .
H7 H 0.372(7) 0.469(3) 0.270(2) 0.020 Uiso 1 1 d . . .
N1 N 0.3305(6) 0.2300(2) 0.42610(17) 0.0217(5) Uani 1 1 d . . .
H1A H 0.433(9) 0.241(4) 0.390(3) 0.061(15) Uiso 1 1 d . . .
H1B H 0.220(8) 0.269(4) 0.406(3) 0.040(12) Uiso 1 1 d . . .
H1C H 0.354(9) 0.268(4) 0.482(3) 0.052(13) Uiso 1 1 d . . .
C1 C 0.6759(5) 0.5291(2) 0.30734(16) 0.0117(5) Uani 1 1 d . . .
C2 C 0.7733(6) 0.5227(3) 0.22466(17) 0.0184(6) Uani 1 1 d . . .
H2C H 0.959(7) 0.530(3) 0.236(2) 0.025(9) Uiso 1 1 d . . .
H2B H 0.696(7) 0.581(3) 0.182(2) 0.024(9) Uiso 1 1 d . . .
H2A H 0.725(8) 0.456(3) 0.200(3) 0.035(11) Uiso 1 1 d . . .
C3 C 0.2914(6) 0.1106(3) 0.4406(2) 0.0266(7) Uani 1 1 d . . .
H3A H 0.159(8) 0.102(4) 0.467(3) 0.037(11) Uiso 1 1 d . . .
H3B H 0.264(9) 0.068(4) 0.390(3) 0.053(14) Uiso 1 1 d . . .
C4 C 0.5206(7) 0.0605(2) 0.4886(2) 0.0273(7) Uani 1 1 d . . .
H4B H 0.573(8) 0.106(3) 0.537(3) 0.033(10) Uiso 1 1 d . . .
H4A H 0.677(8) 0.061(3) 0.456(3) 0.041(12) Uiso 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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 5 -5
-1 4 -2
-2 2 6
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
O1 Zn1 O2 100.06(8) 3_666 1_455 ?
O1 Zn1 O4 90.29(8) 3_666 . ?
O2 Zn1 O4 164.16(8) 1_455 . ?
O1 Zn1 O5 105.93(8) 3_666 1_455 ?
O2 Zn1 O5 93.85(8) 1_455 1_455 ?
O4 Zn1 O5 94.80(8) . 1_455 ?
O1 Zn1 O7 151.98(8) 3_666 . ?
O2 Zn1 O7 86.05(8) 1_455 . ?
O4 Zn1 O7 79.30(7) . . ?
O5 Zn1 O7 100.86(8) 1_455 . ?
O1 Zn1 O1 77.78(8) 3_666 . ?
O2 Zn1 O1 89.99(7) 1_455 . ?
O4 Zn1 O1 80.44(7) . . ?
O5 Zn1 O1 174.07(7) 1_455 . ?
O7 Zn1 O1 74.88(7) . . ?
O2 P1 O1 117.14(12) . . ?
O2 P1 O3 110.01(12) . . ?
O1 P1 O3 107.22(11) . . ?
O2 P1 C1 108.71(11) . . ?
O1 P1 C1 104.41(11) . . ?
O3 P1 C1 109.02(12) . . ?
O5 P2 O4 116.18(12) . . ?
O5 P2 O6 111.41(12) . . ?
O4 P2 O6 107.46(11) . . ?
O5 P2 C1 109.19(12) . . ?
O4 P2 C1 104.96(11) . . ?
O6 P2 C1 107.10(12) . . ?
P1 O1 Zn1 139.52(13) . 3_666 ?
P1 O1 Zn1 113.81(10) . . ?
Zn1 O1 Zn1 102.22(8) 3_666 . ?
H1WB O1W H1WA 103(4) . . ?
P1 O2 Zn1 131.68(12) . 1_655 ?
P1 O3 H3 116(4) . . ?
P2 O4 Zn1 120.00(11) . . ?
P2 O5 Zn1 134.65(12) . 1_655 ?
C1 O7 Zn1 107.27(15) . . ?
C1 O7 H7 107(3) . . ?
Zn1 O7 H7 125(3) . . ?
C3 N1 H1A 112(3) . . ?
C3 N1 H1B 122(3) . . ?
H1A N1 H1B 100(4) . . ?
C3 N1 H1C 108(3) . . ?
H1A N1 H1C 122(4) . . ?
H1B N1 H1C 95(4) . . ?
O7 C1 C2 111.8(2) . . ?
O7 C1 P1 107.00(17) . . ?
C2 C1 P1 114.54(19) . . ?
O7 C1 P2 103.06(17) . . ?
C2 C1 P2 110.33(19) . . ?
P1 C1 P2 109.44(13) . . ?
C1 C2 H2C 108(2) . . ?
C1 C2 H2B 113(2) . . ?
H2C C2 H2B 111(3) . . ?
C1 C2 H2A 108(3) . . ?
H2C C2 H2A 112(3) . . ?
H2B C2 H2A 104(3) . . ?
N1 C3 C4 110.2(3) . . ?
N1 C3 H3A 109(3) . . ?
C4 C3 H3A 112(3) . . ?
N1 C3 H3B 113(3) . . ?
C4 C3 H3B 104(3) . . ?
H3A C3 H3B 108(4) . . ?
C3 C4 C4 111.5(4) . 3_656 ?
C3 C4 H4B 109(2) . . ?
C4 C4 H4B 112(2) 3_656 . ?
C3 C4 H4A 114(2) . . ?
C4 C4 H4A 106(2) 3_656 . ?
H4B C4 H4A 103(3) . . ?
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 O1 2.0051(19) 3_666 ?
Zn1 O2 2.0083(19) 1_455 ?
Zn1 O4 2.0535(18) . ?
Zn1 O5 2.064(2) 1_455 ?
Zn1 O7 2.278(2) . ?
Zn1 O1 2.479(2) . ?
P1 O2 1.505(2) . ?
P1 O1 1.5112(19) . ?
P1 O3 1.549(2) . ?
P1 C1 1.836(3) . ?
P2 O5 1.509(2) . ?
P2 O4 1.5206(18) . ?
P2 O6 1.535(2) . ?
P2 C1 1.838(3) . ?
O1 Zn1 2.0051(19) 3_666 ?
O1W H1WB 0.84(5) . ?
O1W H1WA 0.95(5) . ?
O2 Zn1 2.0083(19) 1_655 ?
O3 H3 0.96(7) . ?
O5 Zn1 2.064(2) 1_655 ?
O7 C1 1.452(3) . ?
O7 H7 0.79(4) . ?
N1 C3 1.485(4) . ?
N1 H1A 0.88(5) . ?
N1 H1B 0.80(5) . ?
N1 H1C 1.00(5) . ?
C1 C2 1.523(4) . ?
C2 H2C 1.01(4) . ?
C2 H2B 1.04(4) . ?
C2 H2A 0.92(4) . ?
C3 C4 1.507(5) . ?
C3 H3A 0.90(4) . ?
C3 H3B 0.96(5) . ?
C4 C4 1.535(6) 3_656 ?
C4 H4B 0.97(4) . ?
C4 H4A 1.07(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
O7 H7 O1W 0.79(4) 1.88(4) 2.657(3) 171(4) .
O3 H3 O6 0.96(7) 1.48(7) 2.428(3) 168(7) 2_645
N1 H1A O3 0.88(5) 2.01(5) 2.844(3) 157(4) .
N1 H1B O2 0.80(5) 2.12(5) 2.820(3) 147(4) 1_455
N1 H1C O4 1.00(5) 1.74(5) 2.736(3) 173(4) 3_666
O1W H1WB O6 0.84(5) 1.90(5) 2.734(3) 172(5) 2_545
