#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:57:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180457 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/26/7212656.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_7212656
loop_
_publ_author_name
'Feng, Jing-Dong'
'Tang, Shu-Wei'
'Shao, Kui-Zhan'
'Wang, Rong-Shun'
'Yao, Chan'
'Xie, Hai-Ming'
'Su, Zhong-Min'
_publ_section_title
;
 Helical channels, low framework density and structure-directing effect: a
 novel non-centrosymmetric zinc phosphate NIS-4 prepared by ionothermal
 reaction
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3448
_journal_paper_doi               10.1039/c002882g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C6 H14 N2 O8 P2 Zn'
_chemical_formula_weight         369.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   8.8490(7)
_cell_length_b                   13.8690(10)
_cell_length_c                   10.8180(8)
_cell_measurement_reflns_used    164
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.55
_cell_measurement_theta_min      2.83
_cell_volume                     1327.66(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'omega scans'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7573
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.6637
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0245
_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)+(0.0351P)²+0.0044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                2884
_reflns_number_total             3013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002882g.txt
_cod_data_source_block           NIS-4
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7212656
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, 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
_atom_site_refinement_flags
Zn1 Zn 0.03756(3) 0.101162(17) 0.32781(3) 0.02015(8) Uani 1 1 d .
P1 P 0.01052(8) -0.07784(5) 0.12516(6) 0.02192(13) Uani 1 1 d .
P2 P -0.17102(7) 0.28392(4) 0.38000(7) 0.02293(14) Uani 1 1 d .
O5 O -0.1013(2) 0.20657(14) 0.30080(17) 0.0334(5) Uani 1 1 d .
O8 O -0.2725(2) 0.24083(13) 0.48230(18) 0.0295(4) Uani 1 1 d .
O4 O -0.0103(2) -0.04953(15) -0.00696(18) 0.0314(4) Uani 1 1 d .
O2 O -0.1000(3) -0.16304(14) 0.1589(2) 0.0385(5) Uani 1 1 d .
O3 O -0.0160(2) 0.00102(17) 0.2165(2) 0.0381(5) Uani 1 1 d .
O7 O -0.0405(2) 0.34147(17) 0.4476(2) 0.0427(6) Uani 1 1 d .
O1 O 0.1750(2) -0.11776(16) 0.1469(2) 0.0418(5) Uani 1 1 d .
O6 O -0.2571(2) 0.35660(14) 0.30376(19) 0.0342(5) Uani 1 1 d .
N1 N -0.3832(3) -0.2149(2) 0.4371(2) 0.0425(6) Uani 1 1 d .
N2 N -0.3918(3) -0.08446(18) 0.3297(3) 0.0434(6) Uani 1 1 d .
C3 C -0.3321(4) -0.1401(3) 0.5111(4) 0.0525(9) Uani 1 1 d .
H3 H -0.2998 -0.1449 0.5926 0.063 Uiso 1 1 calc R
C1 C -0.4169(4) -0.1786(2) 0.3270(4) 0.0415(6) Uani 1 1 d .
H1 H -0.4522 -0.2134 0.2594 0.050 Uiso 1 1 calc R
C2 C -0.3383(4) -0.0602(3) 0.4431(3) 0.0517(9) Uani 1 1 d .
H2 H -0.3108 0.0014 0.4687 0.062 Uiso 1 1 calc R
C4 C -0.4188(5) -0.0170(3) 0.2264(4) 0.0650(11) Uani 1 1 d .
H4A H -0.3924 0.0472 0.2515 0.097 Uiso 1 1 calc R
H4B H -0.5236 -0.0189 0.2036 0.097 Uiso 1 1 calc R
H4C H -0.3579 -0.0355 0.1568 0.097 Uiso 1 1 calc R
C5 C -0.3964(4) -0.3170(3) 0.4735(3) 0.0518(9) Uani 1 1 d .
H5A H -0.4420 -0.3209 0.5549 0.062 Uiso 1 1 calc R
H5B H -0.4622 -0.3501 0.4158 0.062 Uiso 1 1 calc R
C6 C -0.2520(6) -0.3638(3) 0.4757(6) 0.0871(18) Uani 1 1 d .
H6A H -0.2647 -0.4300 0.4994 0.131 Uiso 1 1 calc R
H6B H -0.1873 -0.3320 0.5341 0.131 Uiso 1 1 calc R
H6C H -0.2072 -0.3608 0.3949 0.131 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
O3 Zn1 O6 111.85(9) . 4
O3 Zn1 O5 107.40(9) . .
O6 Zn1 O5 110.44(9) 4 .
O3 Zn1 O4 106.46(10) . 2
O6 Zn1 O4 110.73(9) 4 2
O5 Zn1 O4 109.84(9) . 2
O3 P1 O4 114.92(14) . .
O3 P1 O1 107.70(12) . .
O4 P1 O1 110.44(13) . .
O3 P1 O2 107.37(13) . .
O4 P1 O2 110.00(12) . .
O1 P1 O2 105.99(13) . .
O5 P2 O6 111.84(11) . .
O5 P2 O8 111.73(11) . .
O6 P2 O8 110.86(11) . .
O5 P2 O7 108.85(13) . .
O6 P2 O7 106.52(12) . .
O8 P2 O7 106.76(13) . .
P2 O5 Zn1 135.56(12) . .
P1 O4 Zn1 143.11(13) . 2_554
P1 O3 Zn1 156.48(14) . .
P2 O6 Zn1 127.27(12) . 4_455
C1 N1 C3 107.9(3) . .
C1 N1 C5 125.9(3) . .
C3 N1 C5 126.1(3) . .
C1 N2 C2 108.8(3) . .
C1 N2 C4 125.5(3) . .
C2 N2 C4 125.7(3) . .
C2 C3 N1 106.9(3) . .
C2 C3 H3 126.5 . .
N1 C3 H3 126.5 . .
N2 C1 N1 108.5(3) . .
N2 C1 H1 125.8 . .
N1 C1 H1 125.8 . .
C3 C2 N2 107.9(3) . .
C3 C2 H2 126.1 . .
N2 C2 H2 126.1 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 N1 111.6(3) . .
C6 C5 H5A 109.3 . .
N1 C5 H5A 109.3 . .
C6 C5 H5B 109.3 . .
N1 C5 H5B 109.3 . .
H5A C5 H5B 108.0 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 1.898(2) .
Zn1 O6 1.9264(19) 4
Zn1 O5 1.9319(19) .
Zn1 O4 1.941(2) 2
P1 O3 1.492(2) .
P1 O4 1.494(2) .
P1 O1 1.575(2) .
P1 O2 1.577(2) .
P2 O5 1.5052(19) .
P2 O6 1.5090(19) .
P2 O8 1.546(2) .
P2 O7 1.583(2) .
O4 Zn1 1.941(2) 2_554
O6 Zn1 1.9264(19) 4_455
N1 C1 1.327(5) .
N1 C3 1.385(5) .
N1 C5 1.474(5) .
N2 C1 1.325(4) .
N2 C2 1.357(5) .
N2 C4 1.477(5) .
C3 C2 1.332(6) .
C3 H3 0.9300 .
C1 H1 0.9300 .
C2 H2 0.9300 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.434(6) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O6 P2 O5 Zn1 172.10(17) . .
O8 P2 O5 Zn1 -63.0(2) . .
O7 P2 O5 Zn1 54.7(2) . .
O3 Zn1 O5 P2 148.02(19) . .
O6 Zn1 O5 P2 -89.8(2) 4 .
O4 Zn1 O5 P2 32.6(2) 2 .
O3 P1 O4 Zn1 -164.1(2) . 2_554
O1 P1 O4 Zn1 73.9(3) . 2_554
O2 P1 O4 Zn1 -42.8(3) . 2_554
O4 P1 O3 Zn1 -99.4(4) . .
O1 P1 O3 Zn1 24.1(5) . .
O2 P1 O3 Zn1 137.9(4) . .
O6 Zn1 O3 P1 16.1(5) 4 .
O5 Zn1 O3 P1 137.4(4) . .
O4 Zn1 O3 P1 -105.0(4) 2 .
O5 P2 O6 Zn1 128.02(16) . 4_455
O8 P2 O6 Zn1 2.6(2) . 4_455
O7 P2 O6 Zn1 -113.17(17) . 4_455
C1 N1 C3 C2 0.6(4) . .
C5 N1 C3 C2 -179.9(3) . .
C2 N2 C1 N1 1.1(4) . .
C4 N2 C1 N1 -178.5(3) . .
C3 N1 C1 N2 -1.1(4) . .
C5 N1 C1 N2 179.5(3) . .
N1 C3 C2 N2 0.0(4) . .
C1 N2 C2 C3 -0.7(4) . .
C4 N2 C2 C3 178.9(4) . .
C1 N1 C5 C6 103.1(5) . .
C3 N1 C5 C6 -76.3(5) . .
