#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:23:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179058 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/20/4302036.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_4302036
loop_
_publ_author_name
'Zhien Lin'
'Hari Pada Nayek'
'Stefanie Dehnen'
_publ_contact_author
;
Dehnen, Stefanie

Fachbereich Chemie der Philipps-Universitaet
Hans-Meerwein-Str.
D-35043 Marburg, Germany
;
_publ_contact_author_email       dehnen@chemie.uni-marburg.de
_publ_contact_author_fax         +6421-2825653
_publ_contact_author_phone       +6421-2825751
_publ_section_title
;
Transformation of a Layered Zinc Phosphite to a Three-Dimensional
Open-Framework Structure with Intersecting 16- and 12-Ring Channels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3517
_journal_page_last               3519
_journal_paper_doi               10.1021/ic900306t
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C13 H32 N2 O12 P4 Zn3'
_chemical_formula_weight         728.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.943(3)
_cell_length_b                   15.093(3)
_cell_length_c                   18.521(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2499.9(11)
_computing_cell_refinement       'XAREA 1.38 (Stoe 2006)'
_computing_data_collection       'XAREA 1.38 (Stoe 2006)'
_computing_data_reduction        'XAREA 1.38 (Stoe 2006)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  IPDS-I(Stoe)
_diffrn_measurement_method       'omega scan'
_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  0.0738
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37019
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.171
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0262
_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)+(0.0408P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                2263
_reflns_number_total             2757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900306t_si_002_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2499.8(11)
_cod_database_code               4302036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.39730(3) 0.104817(18) 0.568988(15) 0.01943(9) Uani 1 1 d . . .
Zn2 Zn -0.20562(4) 0.2500 0.49847(2) 0.01873(10) Uani 1 2 d S . .
P1 P 0.59207(7) 0.10292(4) 0.42318(3) 0.01890(14) Uani 1 1 d . . .
H1 H 0.5681(8) 0.1565(18) 0.3667(19) 0.080 Uiso 1 1 calc R . .
P2 P 0.16716(9) 0.2500 0.52933(5) 0.01858(18) Uani 1 2 d S . .
H2 H 0.254(4) 0.2500 0.471(3) 0.080 Uiso 1 2 calc SR . .
P3 P 0.61532(9) 0.2500 0.64681(5) 0.01792(18) Uani 1 2 d S . .
H3 H 0.6526(16) 0.2500 0.719(3) 0.080 Uiso 1 2 calc SR . .
O1 O 0.72856(19) 0.13942(12) 0.46155(10) 0.0247(4) Uani 1 1 d . . .
O2 O 0.6251(2) 0.01239(11) 0.39175(10) 0.0249(4) Uani 1 1 d . . .
O3 O 0.45097(19) 0.10648(12) 0.46816(10) 0.0257(4) Uani 1 1 d . . .
O4 O 0.20258(19) 0.16569(11) 0.57150(10) 0.0225(4) Uani 1 1 d . . .
O5 O 0.0086(3) 0.2500 0.50355(15) 0.0269(6) Uani 1 2 d S . .
O6 O 0.7657(3) 0.2500 0.60633(13) 0.0200(5) Uani 1 2 d S . .
O7 O 0.5310(2) 0.16517(12) 0.63520(10) 0.0252(4) Uani 1 1 d . . .
N1 N -0.0677(2) 0.09238(14) 0.62537(11) 0.0217(4) Uani 1 1 d . . .
H1C H 0.0193 0.0961 0.6011 0.026 Uiso 1 1 calc R . .
H1D H -0.1197 0.1424 0.6169 0.026 Uiso 1 1 calc R . .
C3 C -0.0381(3) -0.08078(16) 0.69531(14) 0.0207(5) Uani 1 1 d . . .
H3A H -0.1328 -0.0836 0.7219 0.025 Uiso 1 1 calc R . .
C1 C -0.0358(3) 0.08578(17) 0.70411(14) 0.0241(5) Uani 1 1 d . . .
H1A H -0.1290 0.0869 0.7309 0.029 Uiso 1 1 calc R . .
H1B H 0.0237 0.1362 0.7192 0.029 Uiso 1 1 calc R . .
C2 C 0.0478(3) 0.00102(16) 0.72072(14) 0.0223(5) Uani 1 1 d . . .
H2A H 0.0644 -0.0030 0.7724 0.027 Uiso 1 1 calc R . .
H2B H 0.1446 0.0025 0.6972 0.027 Uiso 1 1 calc R . .
C5 C -0.1546(3) 0.01491(17) 0.59754(15) 0.0238(5) Uani 1 1 d . . .
H5A H -0.1671 0.0203 0.5457 0.029 Uiso 1 1 calc R . .
H5B H -0.2531 0.0142 0.6195 0.029 Uiso 1 1 calc R . .
C4 C -0.0734(3) -0.07112(17) 0.61489(14) 0.0236(5) Uani 1 1 d . . .
H4A H 0.0192 -0.0733 0.5877 0.028 Uiso 1 1 calc R . .
H4B H -0.1349 -0.1207 0.5997 0.028 Uiso 1 1 calc R . .
C6 C 0.0498(3) -0.16561(16) 0.71060(14) 0.0205(5) Uani 1 1 d . . .
H6A H 0.1379 -0.1666 0.6801 0.025 Uiso 1 1 calc R . .
H6B H 0.0833 -0.1647 0.7604 0.025 Uiso 1 1 calc R . .
C7 C -0.0396(4) -0.2500 0.6978(2) 0.0231(7) Uani 1 2 d S . .
H7A H -0.0761 -0.2500 0.6485 0.028 Uiso 1 2 calc SR . .
H7B H -0.1259 -0.2500 0.7296 0.028 Uiso 1 2 calc SR . .
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
O2 Zn1 O3 113.83(8) 5_656 . ?
O2 Zn1 O7 104.89(8) 5_656 . ?
O3 Zn1 O7 116.93(8) . . ?
O2 Zn1 O4 109.17(7) 5_656 . ?
O3 Zn1 O4 103.70(8) . . ?
O7 Zn1 O4 108.11(8) . . ?
O1 Zn2 O1 123.21(11) 1_455 7_465 ?
O1 Zn2 O5 109.12(6) 1_455 . ?
O1 Zn2 O5 109.12(6) 7_465 . ?
O1 Zn2 O6 108.55(6) 1_455 1_455 ?
O1 Zn2 O6 108.55(6) 7_465 1_455 ?
O5 Zn2 O6 94.49(11) . 1_455 ?
O3 P1 O2 113.97(10) . . ?
O3 P1 O1 113.62(11) . . ?
O2 P1 O1 110.56(10) . . ?
O3 P1 H1 106.0 . . ?
O2 P1 H1 106.0 . . ?
O1 P1 H1 106.0 . . ?
O5 P2 O4 111.10(9) . . ?
O5 P2 O4 111.10(9) . 7_565 ?
O4 P2 O4 112.97(15) . 7_565 ?
O5 P2 H2 107.1 . . ?
O4 P2 H2 107.1 . . ?
O4 P2 H2 107.1 7_565 . ?
O7 P3 O7 117.01(15) . 7_565 ?
O7 P3 O6 111.67(9) . . ?
O7 P3 O6 111.67(9) 7_565 . ?
O7 P3 H3 105.1 . . ?
O7 P3 H3 105.1 7_565 . ?
O6 P3 H3 105.1 . . ?
P1 O1 Zn2 137.59(12) . 1_655 ?
P1 O2 Zn1 131.64(12) . 5_656 ?
P1 O3 Zn1 137.76(11) . . ?
P2 O4 Zn1 124.09(11) . . ?
P2 O5 Zn2 164.20(19) . . ?
P3 O6 Zn2 126.44(14) . 1_655 ?
P3 O7 Zn1 143.18(12) . . ?
C1 N1 C5 112.6(2) . . ?
C1 N1 H1C 109.1 . . ?
C5 N1 H1C 109.1 . . ?
C1 N1 H1D 109.1 . . ?
C5 N1 H1D 109.1 . . ?
H1C N1 H1D 107.8 . . ?
C2 C3 C6 111.2(2) . . ?
C2 C3 C4 109.1(2) . . ?
C6 C3 C4 111.5(2) . . ?
C2 C3 H3A 108.3 . . ?
C6 C3 H3A 108.3 . . ?
C4 C3 H3A 108.3 . . ?
N1 C1 C2 110.5(2) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 111.9(2) . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C5 C4 110.3(2) . . ?
N1 C5 H5A 109.6 . . ?
C4 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C5 C4 C3 112.7(2) . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C7 C6 C3 113.7(2) . . ?
C7 C6 H6A 108.8 . . ?
C3 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
C3 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 C6 113.6(3) . 7 ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 7 . ?
C6 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 7 . ?
H7A C7 H7B 107.7 . . ?
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 O2 1.9231(18) 5_656 ?
Zn1 O3 1.9283(19) . ?
Zn1 O7 1.9397(18) . ?
Zn1 O4 1.9694(18) . ?
Zn2 O1 1.8972(18) 1_455 ?
Zn2 O1 1.8972(18) 7_465 ?
Zn2 O5 1.918(2) . ?
Zn2 O6 2.014(2) 1_455 ?
P1 O3 1.5129(18) . ?
P1 O2 1.5142(18) . ?
P1 O1 1.5160(18) . ?
P1 H1 1.3391 . ?
P2 O5 1.497(2) . ?
P2 O4 1.5263(18) . ?
P2 O4 1.5263(18) 7_565 ?
P2 H2 1.3250 . ?
P3 O7 1.5016(18) . ?
P3 O7 1.5016(18) 7_565 ?
P3 O6 1.540(2) . ?
P3 H3 1.3746 . ?
O1 Zn2 1.8972(18) 1_655 ?
O2 Zn1 1.9231(18) 5_656 ?
O6 Zn2 2.014(2) 1_655 ?
N1 C1 1.489(3) . ?
N1 C5 1.496(3) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
C3 C2 1.528(3) . ?
C3 C6 1.529(3) . ?
C3 C4 1.530(4) . ?
C3 H3A 0.9800 . ?
C1 C2 1.513(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 C4 1.522(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.522(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C6 1.522(3) 7 ?
C7 H7A 0.9700 . ?
C7 H7B 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
N1 H1C O4 0.90 2.02 2.839(3) 150.3 .
N1 H1D O6 0.90 1.93 2.829(2) 175.7 1_455
