#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321360.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_4321360
loop_
_publ_author_name
'Amitava Choudhury'
'Srinivasan Natarajan'
'C. N. R. Rao'
_publ_section_title
;
 Formation of One-, Two-, and Three-Dimensional Open-Framework Zinc
 Phosphates in the Presence of a Tetramine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4295
_journal_page_last               4304
_journal_paper_doi               10.1021/ic000366c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C3 H11 N2 O8 P2 Zn2'
_chemical_formula_weight         395.82
_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
_cell_angle_alpha                111.941(2)
_cell_angle_beta                 107.957(2)
_cell_angle_gamma                103.649(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0636(9)
_cell_length_b                   8.4566(10)
_cell_length_c                   9.0234(11)
_cell_measurement_temperature    293(2)
_cell_volume                     498.09(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2113
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    5.172
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.639
_exptl_crystal_F_000             394
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_obs          0.0437
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0653P)²+1.1810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1152
_refine_ls_wR_factor_obs         0.1094
_reflns_number_observed          1184
_reflns_number_total             1400
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000366c_3.cif
_cod_data_source_block           CompoundIII
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+1.1810P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+1.1810P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321360
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn -0.29541(10) -0.02043(10) -1.02795(9) 0.0150(3) Uani 1 d . .
Zn2 Zn 0.01991(11) -0.46110(12) -0.72127(11) 0.0227(3) Uani 1 d . .
P1 P -0.3158(2) -0.7188(2) -0.6829(2) 0.0158(4) Uani 1 d . .
P2 P -0.0178(2) -0.2370(3) -0.9536(2) 0.0199(5) Uani 1 d . .
O1 O -0.3266(20) -0.8902(10) -0.8239(14) 0.137(5) Uani 1 d . .
O2 O -0.1957(6) 0.1438(7) -1.1121(6) 0.0252(12) Uani 1 d . .
O3 O -0.1003(7) -0.0876(7) -0.9110(7) 0.0278(12) Uani 1 d . .
O4 O -0.4832(7) -0.2676(10) -1.2675(9) 0.052(2) Uani 1 d . .
O5 O 0.2334(8) -0.2861(9) -0.4924(8) 0.049(2) Uani 1 d . .
O6 O -0.0601(7) -0.3432(9) -0.8575(9) 0.042(2) Uani 1 d . .
O7 O 0.1167(7) -0.6330(7) -0.8438(7) 0.0346(14) Uani 1 d . .
O8 O -0.2015(6) -0.5422(7) -0.6781(6) 0.0233(11) Uani 1 d . .
N2 N 0.5209(9) 0.4040(8) -0.2154(7) 0.0236(14) Uani 1 d . .
H9 H 0.6460(9) 0.4655(8) -0.1770(7) 0.028 Uiso 1 calc R .
H8 H 0.4590(9) 0.4643(8) -0.2585(7) 0.028 Uiso 1 calc R .
N1 N 0.1978(9) 0.2165(9) -0.5929(8) 0.028(2) Uani 1 d . .
H3 H 0.0732(9) 0.1637(9) -0.6621(8) 0.042 Uiso 1 calc R .
H2 H 0.2595(9) 0.2035(9) -0.6603(8) 0.042 Uiso 1 calc R .
H1 H 0.2319(9) 0.3368(9) -0.5222(8) 0.042 Uiso 1 calc R .
C1 C 0.2463(11) 0.1249(10) -0.4820(9) 0.024(2) Uani 1 d . .
H5 H 0.2070(11) -0.0065(10) -0.5593(9) 0.029 Uiso 1 calc R .
H4 H 0.1772(11) 0.1374(10) -0.4102(9) 0.029 Uiso 1 calc R .
C2 C 0.4564(10) 0.2098(10) -0.3622(9) 0.023(2) Uani 1 d . .
H7 H 0.4862(10) 0.1324(10) -0.3103(9) 0.028 Uiso 1 calc R .
H6 H 0.5256(10) 0.2128(10) -0.4327(9) 0.028 Uiso 1 calc R .
C3 C 0.4857(10) 0.4045(10) -0.0632(8) 0.019(2) Uani 1 d . .
H10 H 0.5718(10) 0.3630(10) -0.0011(8) 0.023 Uiso 1 calc R .
H11 H 0.3567(10) 0.3187(10) -0.1070(8) 0.023 Uiso 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
O1 Zn1 O3 95.9(4) 1_565 . ?
O1 Zn1 O2 111.6(3) 1_565 . ?
O3 Zn1 O2 110.7(2) . . ?
O1 Zn1 O4 131.0(4) 1_565 . ?
O3 Zn1 O4 104.1(2) . . ?
O2 Zn1 O4 102.3(2) . . ?
O6 Zn2 O5 111.9(3) . . ?
O6 Zn2 O7 108.4(3) . . ?
O5 Zn2 O7 104.6(3) . . ?
O6 Zn2 O8 101.6(2) . . ?
O5 Zn2 O8 107.4(2) . . ?
O7 Zn2 O8 123.0(2) . . ?
O1 P1 O5 108.9(5) . 2_544 ?
O1 P1 O4 106.2(6) . 2_443 ?
O5 P1 O4 110.8(3) 2_544 2_443 ?
O1 P1 O8 112.0(4) . . ?
O5 P1 O8 111.5(3) 2_544 . ?
O4 P1 O8 107.3(3) 2_443 . ?
O6 P2 O2 110.5(3) . 2_553 ?
O6 P2 O7 110.5(3) . 2_543 ?
O2 P2 O7 110.8(3) 2_553 2_543 ?
O6 P2 O3 106.8(3) . . ?
O2 P2 O3 109.6(3) 2_553 . ?
O7 P2 O3 108.6(3) 2_543 . ?
P1 O1 Zn1 153.1(5) . 1_545 ?
P2 O2 Zn1 120.1(3) 2_553 . ?
P2 O3 Zn1 140.4(3) . . ?
P1 O4 Zn1 110.1(4) 2_443 . ?
P1 O5 Zn2 135.3(4) 2_544 . ?
P2 O6 Zn2 149.3(3) . . ?
P2 O7 Zn2 123.2(3) 2_543 . ?
P1 O8 Zn2 135.9(3) . . ?
C3 N2 C2 112.1(5) . . ?
C3 N2 H9 109.2(4) . . ?
C2 N2 H9 109.2(4) . . ?
C3 N2 H8 109.2(4) . . ?
C2 N2 H8 109.2(4) . . ?
H9 N2 H8 107.9 . . ?
C1 N1 H3 109.5(4) . . ?
C1 N1 H2 109.5(4) . . ?
H3 N1 H2 109.5 . . ?
C1 N1 H1 109.5(4) . . ?
H3 N1 H1 109.5 . . ?
H2 N1 H1 109.5 . . ?
N1 C1 C2 111.4(6) . . ?
N1 C1 H5 109.3(4) . . ?
C2 C1 H5 109.3(4) . . ?
N1 C1 H4 109.3(4) . . ?
C2 C1 H4 109.3(4) . . ?
H5 C1 H4 108.0 . . ?
N2 C2 C1 112.4(6) . . ?
N2 C2 H7 109.1(4) . . ?
C1 C2 H7 109.1(4) . . ?
N2 C2 H6 109.1(4) . . ?
C1 C2 H6 109.1(4) . . ?
H7 C2 H6 107.9 . . ?
N2 C3 C3 110.7(7) . 2_665 ?
N2 C3 H10 109.5(4) . . ?
C3 C3 H10 109.5(5) 2_665 . ?
N2 C3 H11 109.5(4) . . ?
C3 C3 H11 109.5(6) 2_665 . ?
H10 C3 H11 108.1 . . ?
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 1.889(6) 1_565 ?
Zn1 O3 1.939(5) . ?
Zn1 O2 1.947(5) . ?
Zn1 O4 2.109(7) . ?
Zn2 O6 1.911(5) . ?
Zn2 O5 1.934(5) . ?
Zn2 O7 1.952(5) . ?
Zn2 O8 1.965(5) . ?
P1 O1 1.490(7) . ?
P1 O5 1.495(5) 2_544 ?
P1 O4 1.505(6) 2_443 ?
P1 O8 1.536(5) . ?
P2 O6 1.515(6) . ?
P2 O2 1.522(5) 2_553 ?
P2 O7 1.540(5) 2_543 ?
P2 O3 1.542(5) . ?
O1 Zn1 1.889(6) 1_545 ?
O2 P2 1.522(5) 2_553 ?
O4 P1 1.505(6) 2_443 ?
O5 P1 1.495(5) 2_544 ?
O7 P2 1.540(5) 2_543 ?
N2 C3 1.484(9) . ?
N2 C2 1.506(9) . ?
N2 H9 0.90 . ?
N2 H8 0.90 . ?
N1 C1 1.494(9) . ?
N1 H3 0.89 . ?
N1 H2 0.89 . ?
N1 H1 0.89 . ?
C1 C2 1.507(10) . ?
C1 H5 0.97 . ?
C1 H4 0.97 . ?
C2 H7 0.97 . ?
C2 H6 0.97 . ?
C3 C3 1.499(13) 2_665 ?
C3 H10 0.97 . ?
C3 H11 0.97 . ?
