#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332180.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332180
loop_
_publ_author_name
'Chen, Lan'
'Bu, Xianhui'
_publ_section_title
;
 (3,4)-Connected Zincophosphites as Structural Analogues of Zinc Hydrogen
 Phosphate
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4654
_journal_page_last               4660
_journal_paper_doi               10.1021/ic060059s
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C4 H20 N2 O12 P4 Zn3'
_chemical_formula_weight         608.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.3570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7891(3)
_cell_length_b                   8.4306(2)
_cell_length_c                   16.1358(5)
_cell_measurement_temperature    273(2)
_cell_volume                     1986.41(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10821
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.969
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0390
_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)+(0.0449P)²+0.8172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                1485
_reflns_number_total             2318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060059ssup3.cif
_cod_data_source_block           test
_cod_database_code               4332180
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Zn1 Zn 0.5000 0.62722(9) 0.2500 0.0397(2) Uani 1 2 d S
Zn2 Zn 0.36356(3) 0.36246(6) 0.47553(3) 0.04009(17) Uani 1 1 d .
P1 P 0.52040(8) 0.37261(13) 0.40048(8) 0.0380(3) Uani 1 1 d .
O1 O 0.6077(2) 0.4220(4) 0.4762(2) 0.0518(8) Uani 1 1 d .
O2 O 0.4557(2) 0.2866(4) 0.4325(2) 0.0534(9) Uani 1 1 d .
O3 O 0.4748(2) 0.5110(4) 0.3406(2) 0.0595(9) Uani 1 1 d .
H1P H 0.548(2) 0.262(4) 0.353(2) 0.025(9) Uiso 1 1 d .
P2 P 0.15252(8) 0.36260(14) 0.36492(8) 0.0402(3) Uani 1 1 d .
H2P H 0.114(3) 0.501(5) 0.344(3) 0.055(13) Uiso 1 1 d .
O4 O 0.2493(2) 0.4002(5) 0.3761(2) 0.0652(11) Uani 1 1 d .
O5 O 0.1397(2) 0.3088(4) 0.4481(2) 0.0531(9) Uani 1 1 d .
O6 O 0.1102(2) 0.2529(5) 0.2863(2) 0.0681(11) Uani 1 1 d .
N1 N 0.1606(3) 0.2810(5) 0.1363(3) 0.0504(10) Uiso 1 1 d .
H1A H 0.1437 0.2091 0.0917 0.061 Uiso 1 1 calc .
H1B H 0.1465 0.2415 0.1812 0.061 Uiso 1 1 calc .
C1 C 0.2607(4) 0.3054(8) 0.1686(4) 0.0815(18) Uiso 1 1 d .
H1A H 0.2763 0.3450 0.1205 0.122 Uiso 1 1 calc R
H1B H 0.2914 0.2063 0.1893 0.122 Uiso 1 1 calc R
H1C H 0.2792 0.3806 0.2169 0.122 Uiso 1 1 calc R
C2 C 0.1087(4) 0.4280(7) 0.1036(4) 0.0737(17) Uiso 1 1 d .
H2A H 0.1214 0.5012 0.1524 0.111 Uiso 1 1 calc R
H2B H 0.0444 0.4046 0.0786 0.111 Uiso 1 1 calc R
H2C H 0.1264 0.4744 0.0582 0.111 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
O O 0.0106 0.0060 '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'
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'
C C 0.0033 0.0016 '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'
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 O3 118.8(2) 2_655 .
O3 Zn1 O6 118.24(14) 2_655 4
O3 Zn1 O6 94.96(15) . 4
O3 Zn1 O6 94.96(15) 2_655 3
O3 Zn1 O6 118.23(14) . 3
O6 Zn1 O6 113.4(3) 4 3
O5 Zn2 O4 114.48(15) 7_556 .
O5 Zn2 O2 100.93(13) 7_556 .
O4 Zn2 O2 110.32(15) . .
O5 Zn2 O1 120.15(14) 7_556 5_666
O4 Zn2 O1 100.33(15) . 5_666
O2 Zn2 O1 110.80(14) . 5_666
O2 P1 O3 111.9(2) . .
O2 P1 O1 112.8(2) . .
O3 P1 O1 111.73(19) . .
O2 P1 H1P 105.3(15) . .
O3 P1 H1P 110.1(15) . .
O1 P1 H1P 104.6(15) . .
P1 O1 Zn2 125.34(19) . 5_666
P1 O2 Zn2 131.8(2) . .
P1 O3 Zn1 133.9(2) . .
O5 P2 O4 115.6(2) . .
O5 P2 O6 113.6(2) . .
O4 P2 O6 109.6(2) . .
O5 P2 H2P 107.4(18) . .
O4 P2 H2P 101.1(19) . .
O6 P2 H2P 108.5(19) . .
P2 O4 Zn2 130.6(2) . .
P2 O5 Zn2 148.3(2) . 7_556
P2 O6 Zn1 130.8(2) . 3_445
C2 N1 C1 112.6(4) . .
C2 N1 H1A 109.1 . .
C1 N1 H1A 109.1 . .
C2 N1 H1B 109.1 . .
C1 N1 H1B 109.1 . .
H1A N1 H1B 107.8 . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 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 1.923(3) 2_655
Zn1 O3 1.923(3) .
Zn1 O6 1.928(3) 4
Zn1 O6 1.928(3) 3
Zn2 O5 1.912(3) 7_556
Zn2 O4 1.930(3) .
Zn2 O2 1.944(3) .
Zn2 O1 1.961(3) 5_666
P1 O2 1.495(3) .
P1 O3 1.511(4) .
P1 O1 1.512(3) .
P1 H1P 1.37(3) .
O1 Zn2 1.961(3) 5_666
P2 O5 1.501(3) .
P2 O4 1.503(3) .
P2 O6 1.506(4) .
P2 H2P 1.30(5) .
O5 Zn2 1.912(3) 7_556
O6 Zn1 1.928(3) 3_445
N1 C2 1.468(6) .
N1 C1 1.478(7) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
