#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:43:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179259 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317946.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_4317946
loop_
_publ_author_name
'Jiang-Gao Mao'
'Zhike Wang'
'Abraham Clearfield'
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Two Divalent Metal
 Diphosphonates with a Layered and a 3D Network Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2334
_journal_page_last               2340
_journal_paper_doi               10.1021/ic011202e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H16 N2 O12 P4 Zn3'
_chemical_formula_weight         628.20
_chemical_name_systematic
;
  ?
;
_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                 94.597(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7788(9)
_cell_length_b                   17.0248(19)
_cell_length_c                   13.0412(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1721.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker Smart CCD'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10632
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.446
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0434
_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)+(0.0686P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                3136
_reflns_number_total             3923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011202e_2.cif
_cod_data_source_block           maoc10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317946
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 0.18872(6) 0.83422(3) 0.35779(4) 0.01334(13) Uani 1 1 d . . .
Zn2 Zn 0.75478(6) 0.60590(3) 0.27977(4) 0.01362(13) Uani 1 1 d . . .
Zn3 Zn 0.05358(6) 0.80665(3) 0.03129(4) 0.01394(13) Uani 1 1 d . . .
P1 P 0.42095(13) 0.70055(6) 0.29124(8) 0.0133(2) Uani 1 1 d . . .
P2 P -0.06463(13) 0.62732(6) 0.06960(8) 0.0132(2) Uani 1 1 d . . .
P3 P 0.92916(13) 0.93046(6) 0.20360(8) 0.0147(2) Uani 1 1 d . . .
P4 P 0.44989(13) 0.80397(6) -0.03571(8) 0.0126(2) Uani 1 1 d . . .
C1 C 0.2879(5) 0.6263(2) 0.2217(3) 0.0150(8) Uani 1 1 d . . .
H1A H 0.3243 0.5748 0.2469 0.018 Uiso 1 1 calc R . .
H1B H 0.1691 0.6336 0.2374 0.018 Uiso 1 1 calc R . .
C2 C 0.1457(5) 0.5848(2) 0.0498(3) 0.0153(8) Uani 1 1 d . . .
H2A H 0.1470 0.5305 0.0725 0.018 Uiso 1 1 calc R . .
H2B H 0.1615 0.5850 -0.0232 0.018 Uiso 1 1 calc R . .
C3 C 0.4587(5) 0.5934(3) 0.0725(3) 0.0184(9) Uani 1 1 d . . .
H3A H 0.5555 0.6199 0.1073 0.028 Uiso 1 1 calc R . .
H3B H 0.4617 0.6000 -0.0005 0.028 Uiso 1 1 calc R . .
H3C H 0.4639 0.5385 0.0891 0.028 Uiso 1 1 calc R . .
C4 C 0.7371(5) 0.8741(3) 0.2338(3) 0.0185(9) Uani 1 1 d . . .
H4A H 0.7748 0.8208 0.2497 0.022 Uiso 1 1 calc R . .
H4B H 0.6977 0.8960 0.2965 0.022 Uiso 1 1 calc R . .
C5 C 0.6276(5) 0.8293(2) 0.0590(3) 0.0162(8) Uani 1 1 d . . .
H5A H 0.6902 0.7814 0.0778 0.019 Uiso 1 1 calc R . .
H5B H 0.7060 0.8636 0.0260 0.019 Uiso 1 1 calc R . .
C6 C 0.4896(6) 0.9453(2) 0.1377(3) 0.0203(9) Uani 1 1 d . . .
H6A H 0.3934 0.9381 0.0877 0.030 Uiso 1 1 calc R . .
H6B H 0.5677 0.9831 0.1125 0.030 Uiso 1 1 calc R . .
H6C H 0.4490 0.9640 0.2009 0.030 Uiso 1 1 calc R . .
N1 N 0.2946(4) 0.62757(19) 0.1061(3) 0.0134(7) Uani 1 1 d . . .
H11A H 0.2894 0.6786 0.0855 0.016 Uiso 1 1 calc R . .
N2 N 0.5813(4) 0.8685(2) 0.1563(3) 0.0162(7) Uani 1 1 d . . .
H12A H 0.5052 0.8360 0.1846 0.019 Uiso 1 1 calc R . .
O1 O 0.4115(4) 0.67899(17) 0.4031(2) 0.0168(6) Uani 1 1 d . . .
O2 O 0.6017(4) 0.69689(16) 0.2539(2) 0.0152(6) Uani 1 1 d . . .
O3 O 0.3416(4) 0.78175(16) 0.2652(2) 0.0145(6) Uani 1 1 d . . .
O4 O -0.0337(4) 0.71319(16) 0.0986(2) 0.0167(6) Uani 1 1 d . . .
O5 O -0.1713(4) 0.61388(17) -0.0318(2) 0.0190(6) Uani 1 1 d . . .
O6 O -0.1320(4) 0.58023(16) 0.1578(2) 0.0162(6) Uani 1 1 d . . .
O7 O 1.0496(4) 0.92045(17) 0.3009(2) 0.0192(6) Uani 1 1 d . . .
O8 O 1.0039(4) 0.89677(18) 0.1088(2) 0.0222(7) Uani 1 1 d . . .
O9 O 0.8777(4) 1.01525(16) 0.1861(2) 0.0172(6) Uani 1 1 d . . .
O10 O 0.2974(4) 0.77893(17) 0.0254(2) 0.0155(6) Uani 1 1 d . . .
O11 O 0.4100(4) 0.87705(17) -0.0994(2) 0.0186(6) Uani 1 1 d . . .
O12 O 0.5153(4) 0.73594(17) -0.0966(2) 0.0182(6) Uani 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
O12 Zn1 O7 101.77(13) 4_576 1_455 ?
O12 Zn1 O5 114.58(13) 4_576 4_676 ?
O7 Zn1 O5 101.63(12) 1_455 4_676 ?
O12 Zn1 O3 112.23(12) 4_576 . ?
O7 Zn1 O3 117.02(12) 1_455 . ?
O5 Zn1 O3 109.24(12) 4_676 . ?
O9 Zn2 O11 104.06(13) 2_645 4_676 ?
O9 Zn2 O6 107.27(12) 2_645 1_655 ?
O11 Zn2 O6 114.25(13) 4_676 1_655 ?
O9 Zn2 O2 110.05(12) 2_645 . ?
O11 Zn2 O2 110.64(12) 4_676 . ?
O6 Zn2 O2 110.30(12) 1_655 . ?
O8 Zn3 O1 103.34(13) 1_455 4_575 ?
O8 Zn3 O10 117.07(13) 1_455 . ?
O1 Zn3 O10 118.76(12) 4_575 . ?
O8 Zn3 O4 108.97(13) 1_455 . ?
O1 Zn3 O4 107.04(13) 4_575 . ?
O10 Zn3 O4 101.10(12) . . ?
O1 P1 O2 114.55(17) . . ?
O1 P1 O3 112.41(16) . . ?
O2 P1 O3 109.23(16) . . ?
O1 P1 C1 103.98(17) . . ?
O2 P1 C1 108.24(17) . . ?
O3 P1 C1 108.06(18) . . ?
O5 P2 O4 115.10(17) . . ?
O5 P2 O6 112.26(17) . . ?
O4 P2 O6 111.91(16) . . ?
O5 P2 C2 104.49(18) . . ?
O4 P2 C2 106.86(17) . . ?
O6 P2 C2 105.27(18) . . ?
O9 P3 O8 110.59(18) . . ?
O9 P3 O7 111.72(17) . . ?
O8 P3 O7 112.67(18) . . ?
O9 P3 C4 108.67(18) . . ?
O8 P3 C4 110.27(19) . . ?
O7 P3 C4 102.60(18) . . ?
O11 P4 O12 113.79(17) . . ?
O11 P4 O10 112.23(17) . . ?
O12 P4 O10 111.35(16) . . ?
O11 P4 C5 106.71(18) . . ?
O12 P4 C5 105.47(18) . . ?
O10 P4 C5 106.68(18) . . ?
N1 C1 P1 114.9(3) . . ?
N1 C2 P2 113.7(3) . . ?
N2 C4 P3 120.5(3) . . ?
N2 C5 P4 117.1(3) . . ?
C3 N1 C2 108.0(3) . . ?
C3 N1 C1 112.6(3) . . ?
C2 N1 C1 113.0(3) . . ?
C6 N2 C5 113.1(3) . . ?
C6 N2 C4 113.4(3) . . ?
C5 N2 C4 111.0(3) . . ?
P1 O1 Zn3 136.98(18) . 4_676 ?
P1 O2 Zn2 122.55(16) . . ?
P1 O3 Zn1 121.40(16) . . ?
P2 O4 Zn3 136.00(18) . . ?
P2 O5 Zn1 143.97(19) . 4_575 ?
P2 O6 Zn2 135.10(18) . 1_455 ?
P3 O7 Zn1 133.67(18) . 1_655 ?
P3 O8 Zn3 147.9(2) . 1_655 ?
P3 O9 Zn2 150.51(19) . 2_655 ?
P4 O10 Zn3 137.76(18) . . ?
P4 O11 Zn2 131.24(18) . 4_575 ?
P4 O12 Zn1 155.0(2) . 4_675 ?
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 O12 1.931(3) 4_576 ?
Zn1 O7 1.936(3) 1_455 ?
Zn1 O5 1.947(3) 4_676 ?
Zn1 O3 1.975(3) . ?
Zn2 O9 1.927(3) 2_645 ?
Zn2 O11 1.929(3) 4_676 ?
Zn2 O6 1.929(3) 1_655 ?
Zn2 O2 1.966(3) . ?
Zn3 O8 1.894(3) 1_455 ?
Zn3 O1 1.944(3) 4_575 ?
Zn3 O10 1.962(3) . ?
Zn3 O4 1.965(3) . ?
P1 O1 1.512(3) . ?
P1 O2 1.526(3) . ?
P1 O3 1.541(3) . ?
P1 C1 1.828(4) . ?
P2 O5 1.521(3) . ?
P2 O4 1.524(3) . ?
P2 O6 1.529(3) . ?
P2 C2 1.826(4) . ?
P3 O9 1.511(3) . ?
P3 O8 1.520(3) . ?
P3 O7 1.525(3) . ?
P3 C4 1.845(4) . ?
P4 O11 1.514(3) . ?
P4 O12 1.515(3) . ?
P4 O10 1.541(3) . ?
P4 C5 1.830(4) . ?
C1 N1 1.513(5) . ?
C2 N1 1.508(5) . ?
C3 N1 1.499(5) . ?
C4 N2 1.517(5) . ?
C5 N2 1.503(5) . ?
C6 N2 1.501(5) . ?
O1 Zn3 1.944(3) 4_676 ?
O5 Zn1 1.946(3) 4_575 ?
O6 Zn2 1.929(3) 1_455 ?
O7 Zn1 1.936(3) 1_655 ?
O8 Zn3 1.894(3) 1_655 ?
O9 Zn2 1.927(3) 2_655 ?
O11 Zn2 1.929(3) 4_575 ?
O12 Zn1 1.931(3) 4_675 ?
