#------------------------------------------------------------------------------
#$Date: 2018-08-26 19:36:40 +0300 (Sun, 26 Aug 2018) $
#$Revision: 210165 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/07/4300776.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_4300776
loop_
_publ_author_name
'Fan, Jian'
'Slebodnick, Carla'
'Troya, Diego'
'Angel, Ross'
'Hanson, Brian E.'
_publ_section_title
;
 Five New Zinc Phosphite Structures: Tertiary Building Blocks
 in the Construction of Hybrid Materials
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2719
_journal_page_last               2727
_journal_paper_doi               10.1021/ic048204u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C14 H16 N4 O6 P2 Zn2'
_chemical_formula_sum            'C14 H16 N4 O6 P2 Zn2'
_chemical_formula_weight         528.99
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.866(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6613(5)
_cell_length_b                   16.3179(11)
_cell_length_c                   14.5275(10)
_cell_measurement_reflns_used    11289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      1.90
_cell_volume                     1813.9(2)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_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      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 2 CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18295
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.863
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0255
_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)+(0.0386P)²+0.2234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                4559
_reflns_number_total             5318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048204usi20041220_011211_5.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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_database_code               4300776
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 0.75274(3) 0.679177(12) 0.680962(13) 0.01024(6) Uani 1 1 d . . .
Zn2 Zn 0.74220(3) 0.483630(12) 0.451542(13) 0.00987(5) Uani 1 1 d . . .
P1 P 0.92225(6) 0.49905(3) 0.65890(3) 0.00984(9) Uani 1 1 d . . .
P2 P 0.53697(6) 0.64527(3) 0.50602(3) 0.00974(9) Uani 1 1 d . . .
O4 O 0.61741(18) 0.58610(8) 0.44032(9) 0.0158(3) Uani 1 1 d . . .
O6 O 0.67043(17) 0.70200(8) 0.55475(9) 0.0136(2) Uani 1 1 d . . .
O2 O 0.84989(17) 0.45841(8) 0.57140(9) 0.0159(3) Uani 1 1 d . . .
O1 O 0.80909(17) 0.56552(8) 0.69733(9) 0.0171(3) Uani 1 1 d . . .
N12 N 0.3374(2) 0.68659(9) 0.84996(10) 0.0112(3) Uani 1 1 d . . .
C12 C 0.4303(2) 0.65920(11) 0.78073(12) 0.0128(3) Uani 1 1 d . . .
H12A H 0.3986 0.6136 0.7429 0.015 Uiso 1 1 calc R . .
C5 C 0.3099(3) 0.50697(12) 1.08038(13) 0.0176(4) Uani 1 1 d . . .
H5A H 0.3569 0.5100 1.1420 0.021 Uiso 1 1 calc R . .
N11 N 0.5726(2) 0.70430(9) 0.77199(10) 0.0125(3) Uani 1 1 d . . .
N32 N 0.3041(2) 0.31858(9) 0.84862(11) 0.0127(3) Uani 1 1 d . . .
C4 C 0.2704(2) 0.43093(12) 1.04124(13) 0.0151(3) Uani 1 1 d . . .
H4A H 0.2923 0.3824 1.0760 0.018 Uiso 1 1 calc R . .
C31 C 0.1598(2) 0.34442(11) 0.90583(14) 0.0162(4) Uani 1 1 d . . .
H31A H 0.1417 0.3025 0.9537 0.019 Uiso 1 1 calc R . .
H31B H 0.0506 0.3488 0.8667 0.019 Uiso 1 1 calc R . .
C11 C 0.1758(2) 0.64968(11) 0.88207(13) 0.0137(3) Uani 1 1 d . . .
H11A H 0.0981 0.6353 0.8280 0.016 Uiso 1 1 calc R . .
H11B H 0.1143 0.6905 0.9191 0.016 Uiso 1 1 calc R . .
C13 C 0.5678(2) 0.76397(11) 0.83974(12) 0.0132(3) Uani 1 1 d . . .
H13A H 0.6527 0.8057 0.8505 0.016 Uiso 1 1 calc R . .
C1 C 0.2107(2) 0.57395(11) 0.93945(12) 0.0116(3) Uani 1 1 d . . .
C2 C 0.1689(2) 0.49755(11) 0.90161(12) 0.0117(3) Uani 1 1 d . . .
H2A H 0.1188 0.4945 0.8406 0.014 Uiso 1 1 calc R . .
C14 C 0.4233(2) 0.75342(11) 0.88806(13) 0.0139(3) Uani 1 1 d . . .
H14A H 0.3880 0.7857 0.9383 0.017 Uiso 1 1 calc R . .
C6 C 0.2811(2) 0.57812(12) 1.03018(13) 0.0154(4) Uani 1 1 d . . .
H6A H 0.3091 0.6298 1.0572 0.018 Uiso 1 1 calc R . .
C33 C 0.5076(3) 0.32058(11) 0.74952(12) 0.0155(4) Uani 1 1 d . . .
H33A H 0.5772 0.3358 0.7000 0.019 Uiso 1 1 calc R . .
C34 C 0.3622(3) 0.36061(12) 0.77438(13) 0.0164(4) Uani 1 1 d . . .
H34A H 0.3112 0.4080 0.7462 0.020 Uiso 1 1 calc R . .
C3 C 0.1990(2) 0.42572(11) 0.95132(12) 0.0122(3) Uani 1 1 d . . .
C32 C 0.4125(2) 0.25506(11) 0.86575(13) 0.0141(3) Uani 1 1 d . . .
H32A H 0.3996 0.2161 0.9135 0.017 Uiso 1 1 calc R . .
O5 O 0.41761(17) 0.60765(8) 0.57432(9) 0.0162(3) Uani 1 1 d . . .
O3 O 1.11097(17) 0.52636(9) 0.65296(9) 0.0195(3) Uani 1 1 d . . .
N31 N 0.5394(2) 0.25402(9) 0.80731(10) 0.0136(3) Uani 1 1 d . . .
H1 H 0.922(2) 0.4409(12) 0.7249(13) 0.005(5) Uiso 1 1 d . . .
H2 H 0.436(3) 0.6942(13) 0.4524(15) 0.011(5) 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_
_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 O6 111.26(6) . . ?
O1 Zn1 N11 105.95(6) . . ?
O6 Zn1 N11 112.46(6) . . ?
O1 Zn1 N31 113.92(6) . 2_656 ?
O6 Zn1 N31 100.48(6) . 2_656 ?
N11 Zn1 N31 112.94(6) . 2_656 ?
O4 Zn2 O2 116.62(6) . . ?
O4 Zn2 O3 108.11(6) . 3_766 ?
O2 Zn2 O3 116.65(6) . 3_766 ?
O4 Zn2 O5 109.98(6) . 3_666 ?
O2 Zn2 O5 104.25(6) . 3_666 ?
O3 Zn2 O5 99.66(6) 3_766 3_666 ?
O1 P1 O2 115.55(8) . . ?
O1 P1 O3 112.04(8) . . ?
O2 P1 O3 112.97(8) . . ?
O1 P1 H1 102.7(8) . . ?
O2 P1 H1 106.0(8) . . ?
O3 P1 H1 106.4(8) . . ?
O4 P2 O5 115.73(8) . . ?
O4 P2 O6 113.30(8) . . ?
O5 P2 O6 110.77(7) . . ?
O4 P2 H2 104.9(9) . . ?
O5 P2 H2 105.8(9) . . ?
O6 P2 H2 105.3(9) . . ?
P2 O4 Zn2 135.79(8) . . ?
P2 O6 Zn1 119.94(7) . . ?
P1 O2 Zn2 141.69(9) . . ?
P1 O1 Zn1 141.07(9) . . ?
C12 N12 C14 107.79(15) . . ?
C12 N12 C11 126.06(15) . . ?
C14 N12 C11 126.11(15) . . ?
N11 C12 N12 110.94(16) . . ?
N11 C12 H12A 124.5 . . ?
N12 C12 H12A 124.5 . . ?
C6 C5 C4 120.50(17) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C12 N11 C13 105.68(15) . . ?
C12 N11 Zn1 123.15(12) . . ?
C13 N11 Zn1 131.07(12) . . ?
C32 N32 C34 108.03(16) . . ?
C32 N32 C31 126.08(16) . . ?
C34 N32 C31 125.55(15) . . ?
C3 C4 C5 120.29(17) . . ?
C3 C4 H4A 119.9 . . ?
C5 C4 H4A 119.9 . . ?
N32 C31 C3 111.07(15) . . ?
N32 C31 H31A 109.4 . . ?
C3 C31 H31A 109.4 . . ?
N32 C31 H31B 109.4 . . ?
C3 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
N12 C11 C1 112.45(14) . . ?
N12 C11 H11A 109.1 . . ?
C1 C11 H11A 109.1 . . ?
N12 C11 H11B 109.1 . . ?
C1 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C14 C13 N11 109.34(16) . . ?
C14 C13 H13A 125.3 . . ?
N11 C13 H13A 125.3 . . ?
C2 C1 C6 119.00(17) . . ?
C2 C1 C11 118.99(16) . . ?
C6 C1 C11 122.00(17) . . ?
C3 C2 C1 121.39(17) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C13 C14 N12 106.25(16) . . ?
C13 C14 H14A 126.9 . . ?
N12 C14 H14A 126.9 . . ?
C5 C6 C1 119.94(17) . . ?
C5 C6 H6A 120.0 . . ?
C1 C6 H6A 120.0 . . ?
C34 C33 N31 109.75(17) . . ?
C34 C33 H33A 125.1 . . ?
N31 C33 H33A 125.1 . . ?
C33 C34 N32 105.79(16) . . ?
C33 C34 H34A 127.1 . . ?
N32 C34 H34A 127.1 . . ?
C2 C3 C4 118.86(17) . . ?
C2 C3 C31 119.39(16) . . ?
C4 C3 C31 121.71(17) . . ?
N31 C32 N32 111.00(16) . . ?
N31 C32 H32A 124.5 . . ?
N32 C32 H32A 124.5 . . ?
P2 O5 Zn2 125.25(8) . 3_666 ?
P1 O3 Zn2 127.60(8) . 3_766 ?
C32 N31 C33 105.43(15) . . ?
C32 N31 Zn1 123.98(12) . 2_646 ?
C33 N31 Zn1 129.97(13) . 2_646 ?
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 1.9163(13) . ?
Zn1 O6 1.9449(13) . ?
Zn1 N11 2.0009(15) . ?
Zn1 N31 2.0074(15) 2_656 ?
Zn2 O4 1.9290(13) . ?
Zn2 O2 1.9335(13) . ?
Zn2 O3 1.9410(13) 3_766 ?
Zn2 O5 1.9527(13) 3_666 ?
P1 O1 1.5127(13) . ?
P1 O2 1.5141(13) . ?
P1 O3 1.5195(14) . ?
P1 H1 1.35(2) . ?
P2 O4 1.5106(13) . ?
P2 O5 1.5128(14) . ?
P2 O6 1.5267(13) . ?
P2 H2 1.34(2) . ?
N12 C12 1.338(2) . ?
N12 C14 1.376(2) . ?
N12 C11 1.473(2) . ?
C12 N11 1.327(2) . ?
C12 H12A 0.9500 . ?
C5 C6 1.383(3) . ?
C5 C4 1.392(3) . ?
C5 H5A 0.9500 . ?
N11 C13 1.386(2) . ?
N32 C32 1.344(2) . ?
N32 C34 1.371(2) . ?
N32 C31 1.478(2) . ?
C4 C3 1.394(2) . ?
C4 H4A 0.9500 . ?
C31 C3 1.506(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C11 C1 1.507(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.351(3) . ?
C13 H13A 0.9500 . ?
C1 C2 1.393(2) . ?
C1 C6 1.401(2) . ?
C2 C3 1.390(2) . ?
C2 H2A 0.9500 . ?
C14 H14A 0.9500 . ?
C6 H6A 0.9500 . ?
C33 C34 1.356(3) . ?
C33 N31 1.387(2) . ?
C33 H33A 0.9500 . ?
C34 H34A 0.9500 . ?
C32 N31 1.323(2) . ?
C32 H32A 0.9500 . ?
O5 Zn2 1.9527(13) 3_666 ?
O3 Zn2 1.9410(13) 3_766 ?
N31 Zn1 2.0074(15) 2_646 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 P2 O4 Zn2 -49.84(14) . . . . ?
O6 P2 O4 Zn2 79.67(13) . . . . ?
O2 Zn2 O4 P2 -20.24(15) . . . . ?
O3 Zn2 O4 P2 -154.01(12) 3_766 . . . ?
O5 Zn2 O4 P2 98.13(13) 3_666 . . . ?
O4 P2 O6 Zn1 -101.05(9) . . . . ?
O5 P2 O6 Zn1 30.93(11) . . . . ?
O1 Zn1 O6 P2 45.23(10) . . . . ?
N11 Zn1 O6 P2 -73.45(10) . . . . ?
N31 Zn1 O6 P2 166.19(9) 2_656 . . . ?
O1 P1 O2 Zn2 46.45(16) . . . . ?
O3 P1 O2 Zn2 -84.43(15) . . . . ?
O4 Zn2 O2 P1 -25.28(16) . . . . ?
O3 Zn2 O2 P1 104.55(14) 3_766 . . . ?
O5 Zn2 O2 P1 -146.72(13) 3_666 . . . ?
O2 P1 O1 Zn1 -81.22(16) . . . . ?
O3 P1 O1 Zn1 50.10(17) . . . . ?
O6 Zn1 O1 P1 55.94(16) . . . . ?
N11 Zn1 O1 P1 178.46(14) . . . . ?
N31 Zn1 O1 P1 -56.78(16) 2_656 . . . ?
C14 N12 C12 N11 0.3(2) . . . . ?
C11 N12 C12 N11 -177.35(16) . . . . ?
N12 C12 N11 C13 -0.4(2) . . . . ?
N12 C12 N11 Zn1 176.40(11) . . . . ?
O1 Zn1 N11 C12 -49.96(15) . . . . ?
O6 Zn1 N11 C12 71.79(15) . . . . ?
N31 Zn1 N11 C12 -175.33(14) 2_656 . . . ?
O1 Zn1 N11 C13 125.90(16) . . . . ?
O6 Zn1 N11 C13 -112.35(16) . . . . ?
N31 Zn1 N11 C13 0.53(18) 2_656 . . . ?
C6 C5 C4 C3 -0.9(3) . . . . ?
C32 N32 C31 C3 111.69(19) . . . . ?
C34 N32 C31 C3 -60.8(2) . . . . ?
C12 N12 C11 C1 76.9(2) . . . . ?
C14 N12 C11 C1 -100.4(2) . . . . ?
C12 N11 C13 C14 0.2(2) . . . . ?
Zn1 N11 C13 C14 -176.16(13) . . . . ?
N12 C11 C1 C2 -106.96(18) . . . . ?
N12 C11 C1 C6 74.1(2) . . . . ?
C6 C1 C2 C3 -1.3(3) . . . . ?
C11 C1 C2 C3 179.72(16) . . . . ?
N11 C13 C14 N12 0.0(2) . . . . ?
C12 N12 C14 C13 -0.2(2) . . . . ?
C11 N12 C14 C13 177.51(16) . . . . ?
C4 C5 C6 C1 0.4(3) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C11 C1 C6 C5 179.61(17) . . . . ?
N31 C33 C34 N32 0.3(2) . . . . ?
C32 N32 C34 C33 -0.6(2) . . . . ?
C31 N32 C34 C33 173.00(17) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C1 C2 C3 C31 -177.06(16) . . . . ?
C5 C4 C3 C2 0.3(3) . . . . ?
C5 C4 C3 C31 178.14(17) . . . . ?
N32 C31 C3 C2 81.6(2) . . . . ?
N32 C31 C3 C4 -96.2(2) . . . . ?
C34 N32 C32 N31 0.8(2) . . . . ?
C31 N32 C32 N31 -172.84(16) . . . . ?
O4 P2 O5 Zn2 -36.93(13) . . . 3_666 ?
O6 P2 O5 Zn2 -167.66(9) . . . 3_666 ?
O1 P1 O3 Zn2 -131.35(11) . . . 3_766 ?
O2 P1 O3 Zn2 1.26(15) . . . 3_766 ?
N32 C32 N31 C33 -0.6(2) . . . . ?
N32 C32 N31 Zn1 171.24(12) . . . 2_646 ?
C34 C33 N31 C32 0.1(2) . . . . ?
C34 C33 N31 Zn1 -170.98(13) . . . 2_646 ?
