#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:10:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180379 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/48/7204854.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_7204854
loop_
_publ_author_name
'Lin, Zhi-En'
'Zhang, Jie'
'Zheng, Shou-Tian'
'Yang, Guo-Yu'
_publ_section_title
;
 Synthesis and characterization of a novel open-framework nickel?zinc
 phosphite with intersecting three-dimensional 16-ring channels
;
_journal_issue                   10
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1652
_journal_paper_doi               10.1039/b402321h
_journal_volume                  14
_journal_year                    2004
_chemical_formula_sum            'C4 H18 N3 Ni O10 P3 Zn2'
_chemical_formula_weight         550.57
_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-97
_cell_angle_alpha                102.997(2)
_cell_angle_beta                 94.614(2)
_cell_angle_gamma                115.952(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5848(6)
_cell_length_b                   9.1884(6)
_cell_length_c                   11.9256(8)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      1.79
_cell_volume                     806.81(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4202
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.452
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4245
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0286(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0516P)²+3.0685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                2696
_reflns_number_total             2825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402321h.txt
_cod_data_source_block           2
_cod_original_cell_volume        806.81(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204854
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.0406
#END Tags that were not found in dictionaries
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_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 0.50585(8) 0.23840(7) -0.02556(5) 0.0212(2) Uani 1 1 d . . .
Zn2 Zn 0.53693(7) 0.37852(6) 0.34219(5) 0.0187(2) Uani 1 1 d . . .
Ni1 Ni 1.00808(7) 0.91191(7) 0.36856(5) 0.0163(2) Uani 1 1 d . . .
P1 P 0.35005(17) 0.44077(15) 0.13437(11) 0.0202(3) Uani 1 1 d . . .
H1 H 0.199(7) 0.377(7) 0.169(5) 0.022(13) Uiso 1 1 d . . .
P2 P 0.66091(17) 0.14658(15) 0.18613(11) 0.0200(3) Uani 1 1 d . . .
H2 H 0.819(9) 0.241(8) 0.246(6) 0.045(18) Uiso 1 1 d . . .
P3 P 0.81303(16) 0.68659(14) 0.54436(10) 0.0179(3) Uani 1 1 d . . .
H3 H 0.895(8) 0.682(8) 0.639(5) 0.033(16) Uiso 1 1 d . . .
O1 O 0.3558(6) 0.5865(5) 0.0945(3) 0.0336(9) Uani 1 1 d . . .
O2 O 0.5017(5) 0.5014(5) 0.2377(3) 0.0353(9) Uani 1 1 d . . .
O3 O 0.3323(5) 0.2922(5) 0.0393(4) 0.0357(9) Uani 1 1 d . . .
O4 O 0.6629(5) 0.2093(5) 0.0800(3) 0.0327(9) Uani 1 1 d . . .
O5 O 0.6346(5) -0.0343(5) 0.1579(3) 0.0310(9) Uani 1 1 d . . .
O6 O 0.5346(5) 0.1693(4) 0.2620(3) 0.0308(8) Uani 1 1 d . . .
O7 O 0.7672(5) 0.5351(4) 0.4414(3) 0.0267(8) Uani 1 1 d . . .
O8 O 0.6525(6) 0.6988(5) 0.5765(4) 0.0432(11) Uani 1 1 d . . .
O9 O 0.9483(4) 0.8518(4) 0.5273(3) 0.0177(7) Uani 1 1 d . . .
OW1 O 0.7355(5) 0.8431(5) 0.3222(3) 0.0260(8) Uani 1 1 d . . .
H4 H 0.655(8) 0.743(8) 0.299(5) 0.021(14) Uiso 1 1 d . . .
H5 H 0.697(8) 0.886(8) 0.267(6) 0.033(16) Uiso 1 1 d . . .
N1 N 1.2630(6) 0.9590(6) 0.4286(5) 0.0277(10) Uani 1 1 d . . .
H6 H 1.299(11) 1.028(11) 0.500(8) 0.06(2) Uiso 1 1 d . . .
H7 H 1.343(11) 1.026(10) 0.407(7) 0.05(2) Uiso 1 1 d . . .
N2 N 0.9849(7) 0.6796(6) 0.2762(4) 0.0267(10) Uani 1 1 d . . .
H8 H 0.912(8) 0.630(8) 0.295(5) 0.018(16) Uiso 1 1 d . . .
N3 N 1.0444(7) 0.9653(6) 0.2063(4) 0.0340(11) Uani 1 1 d . . .
H9 H 0.932(10) 0.965(9) 0.165(6) 0.047(19) Uiso 1 1 d . . .
H10 H 1.135(16) 1.061(14) 0.213(10) 0.11(4) Uiso 1 1 d . . .
C1 C 1.2548(17) 0.7986(18) 0.4376(11) 0.029(3) Uani 0.50 1 d P . .
C1' C 1.2876(19) 0.8076(18) 0.3783(18) 0.048(4) Uani 0.50 1 d P . .
C2 C 1.1407(11) 0.6657(9) 0.3215(7) 0.055(2) Uani 1 1 d . . .
C3 C 0.9588(9) 0.6661(8) 0.1504(5) 0.0390(14) Uani 1 1 d . . .
H11 H 0.992(9) 0.577(9) 0.104(6) 0.045(19) Uiso 1 1 d . . .
H12 H 0.823(10) 0.622(9) 0.118(6) 0.047(19) Uiso 1 1 d . . .
C4 C 1.0745(9) 0.8326(8) 0.1299(5) 0.0403(14) Uani 1 1 d . . .
H13 H 1.046(9) 0.832(8) 0.047(6) 0.042(18) Uiso 1 1 d . . .
H14 H 1.198(10) 0.865(9) 0.146(6) 0.044(19) 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'
Ni Ni 0.3393 1.1124 '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 O3 116.69(17) . . ?
O4 Zn1 O1 109.01(17) . 2_665 ?
O3 Zn1 O1 108.41(17) . 2_665 ?
O4 Zn1 O5 112.16(16) . 2_655 ?
O3 Zn1 O5 104.15(17) . 2_655 ?
O1 Zn1 O5 105.79(17) 2_665 2_655 ?
O8 Zn2 O7 115.26(19) 2_666 . ?
O8 Zn2 O6 101.87(16) 2_666 . ?
O7 Zn2 O6 110.06(16) . . ?
O8 Zn2 O2 112.0(2) 2_666 . ?
O7 Zn2 O2 103.89(16) . . ?
O6 Zn2 O2 114.10(16) . . ?
N1 Ni1 N2 82.13(19) . . ?
N1 Ni1 O9 92.81(16) . 2_776 ?
N2 Ni1 O9 174.53(16) . 2_776 ?
N1 Ni1 N3 97.7(2) . . ?
N2 Ni1 N3 82.9(2) . . ?
O9 Ni1 N3 99.91(17) 2_776 . ?
N1 Ni1 OW1 172.34(18) . . ?
N2 Ni1 OW1 95.90(18) . . ?
O9 Ni1 OW1 88.85(14) 2_776 . ?
N3 Ni1 OW1 89.34(18) . . ?
N1 Ni1 O9 87.11(18) . . ?
N2 Ni1 O9 97.44(16) . . ?
O9 Ni1 O9 80.17(13) 2_776 . ?
N3 Ni1 O9 175.15(18) . . ?
OW1 Ni1 O9 85.81(14) . . ?
O1 P1 O3 115.8(2) . . ?
O1 P1 O2 110.9(2) . . ?
O3 P1 O2 112.7(2) . . ?
O1 P1 H1 105(2) . . ?
O3 P1 H1 102(2) . . ?
O2 P1 H1 109(2) . . ?
O4 P2 O6 114.3(2) . . ?
O4 P2 O5 113.6(2) . . ?
O6 P2 O5 111.1(2) . . ?
O4 P2 H2 103(3) . . ?
O6 P2 H2 108(3) . . ?
O5 P2 H2 106(3) . . ?
O8 P3 O7 112.8(2) . . ?
O8 P3 O9 111.3(2) . . ?
O7 P3 O9 112.69(19) . . ?
O8 P3 H3 106(3) . . ?
O7 P3 H3 112(3) . . ?
O9 P3 H3 102(3) . . ?
P1 O1 Zn1 143.6(3) . 2_665 ?
P1 O2 Zn2 129.0(2) . . ?
P1 O3 Zn1 132.1(3) . . ?
P2 O4 Zn1 138.8(2) . . ?
P2 O5 Zn1 133.6(2) . 2_655 ?
P2 O6 Zn2 127.8(2) . . ?
P3 O7 Zn2 127.6(2) . . ?
P3 O8 Zn2 146.0(3) . 2_666 ?
P3 O9 Ni1 121.91(18) . 2_776 ?
P3 O9 Ni1 129.23(19) . . ?
Ni1 O9 Ni1 99.83(13) 2_776 . ?
Ni1 OW1 H4 124(4) . . ?
Ni1 OW1 H5 120(4) . . ?
H4 OW1 H5 99(5) . . ?
C1 N1 C1' 30.8(7) . . ?
C1 N1 Ni1 107.6(6) . . ?
C1' N1 Ni1 110.8(6) . . ?
C1 N1 H6 107(6) . . ?
C1' N1 H6 130(6) . . ?
Ni1 N1 H6 107(5) . . ?
C1 N1 H7 122(6) . . ?
C1' N1 H7 97(6) . . ?
Ni1 N1 H7 119(6) . . ?
H6 N1 H7 91(7) . . ?
C3 N2 C2 114.4(5) . . ?
C3 N2 Ni1 108.0(4) . . ?
C2 N2 Ni1 109.1(4) . . ?
C3 N2 H8 116(5) . . ?
C2 N2 H8 111(5) . . ?
Ni1 N2 H8 97(5) . . ?
C4 N3 Ni1 108.4(4) . . ?
C4 N3 H9 109(4) . . ?
Ni1 N3 H9 110(4) . . ?
C4 N3 H10 107(7) . . ?
Ni1 N3 H10 113(8) . . ?
H9 N3 H10 109(9) . . ?
C1' C1 N1 76.3(15) . . ?
C1' C1 C2 60.5(16) . . ?
N1 C1 C2 106.0(8) . . ?
C1 C1' C2 88(2) . . ?
C1 C1' N1 72.9(16) . . ?
C2 C1' N1 115.8(10) . . ?
C1' C2 N2 118.3(7) . . ?
C1' C2 C1 31.1(9) . . ?
N2 C2 C1 114.8(6) . . ?
N2 C3 C4 110.8(5) . . ?
N2 C3 H11 111(4) . . ?
C4 C3 H11 107(4) . . ?
N2 C3 H12 108(4) . . ?
C4 C3 H12 112(4) . . ?
H11 C3 H12 107(5) . . ?
N3 C4 C3 108.4(5) . . ?
N3 C4 H13 107(4) . . ?
C3 C4 H13 112(4) . . ?
N3 C4 H14 109(4) . . ?
C3 C4 H14 114(4) . . ?
H13 C4 H14 106(6) . . ?
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 1.915(4) . ?
Zn1 O3 1.929(4) . ?
Zn1 O1 1.937(4) 2_665 ?
Zn1 O5 1.961(4) 2_655 ?
Zn2 O8 1.909(4) 2_666 ?
Zn2 O7 1.936(4) . ?
Zn2 O6 1.936(3) . ?
Zn2 O2 1.947(4) . ?
Ni1 N1 2.067(5) . ?
Ni1 N2 2.084(4) . ?
Ni1 O9 2.097(3) 2_776 ?
Ni1 N3 2.114(5) . ?
Ni1 OW1 2.126(4) . ?
Ni1 O9 2.129(3) . ?
P1 O1 1.502(4) . ?
P1 O3 1.506(4) . ?
P1 O2 1.524(4) . ?
P1 H1 1.32(5) . ?
P2 O4 1.503(4) . ?
P2 O6 1.519(4) . ?
P2 O5 1.528(4) . ?
P2 H2 1.28(7) . ?
P3 O8 1.503(4) . ?
P3 O7 1.508(4) . ?
P3 O9 1.526(3) . ?
P3 H3 1.30(6) . ?
O1 Zn1 1.937(4) 2_665 ?
O5 Zn1 1.961(4) 2_655 ?
O8 Zn2 1.909(4) 2_666 ?
O9 Ni1 2.097(3) 2_776 ?
OW1 H4 0.83(6) . ?
OW1 H5 0.94(7) . ?
N1 C1 1.474(14) . ?
N1 C1' 1.498(14) . ?
N1 H6 0.88(9) . ?
N1 H7 0.81(9) . ?
N2 C3 1.468(7) . ?
N2 C2 1.470(8) . ?
N2 H8 0.68(6) . ?
N3 C4 1.482(8) . ?
N3 H9 1.05(7) . ?
N3 H10 0.86(12) . ?
C1 C1' 0.790(19) . ?
C1 C2 1.530(15) . ?
C1' C2 1.333(16) . ?
C3 C4 1.504(9) . ?
C3 H11 1.04(7) . ?
C3 H12 1.06(7) . ?
C4 H13 1.00(7) . ?
C4 H14 0.95(7) . ?
