#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:26:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179844 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/40/7014026.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_7014026
loop_
_publ_author_name
'Anantharaman, Ganapathi'
'Chandrasekhar, Vadapalli'
'Walawalkar, Mrinalini G.'
'Roesky, Herbert W.'
'Vidovic, Denis'
'Magull, Jorg'
'Noltemeyer, Mathias'
_publ_section_title
;
 Molecular zinc phosphonates: synthesis and X-ray crystal structures of
 [[(ZnMe)4(THF)2][tBuPO3]2] and
 [[(ZnEt)3(Zn(THF))3][tBuPO3]4[mu3-OEt]].
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1271
_journal_page_last               1275
_journal_paper_doi               10.1039/b400168k
_journal_year                    2004
_chemical_formula_sum            'C20 H46 O8 P2 Zn4'
_chemical_formula_weight         737.99
_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                 95.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.933(2)
_cell_length_b                   11.311(2)
_cell_length_c                   13.865(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1550.4(5)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.1860
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3640
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.197
_exptl_absorpt_correction_T_max  0.2500
_exptl_absorpt_correction_T_min  0.1423
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             760
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0744P)²+1.2743P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                2369
_reflns_number_total             2728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400168k.txt
_cod_data_source_block           zincphosphonate(2)
_cod_original_cell_volume        1550.3(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7014026
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 0.19839(6) 0.86883(4) 0.49400(4) 0.0256(2) Uani 1 1 d . . .
P1 P -0.11070(12) 0.86830(9) 0.51912(8) 0.0209(3) Uani 1 1 d . . .
O1 O 0.1972(3) 1.0310(3) 0.4479(2) 0.0247(7) Uani 1 1 d . . .
C1 C 0.2853(6) 0.7280(4) 0.4499(4) 0.0371(12) Uani 1 1 d . . .
H1B H 0.2176 0.6776 0.4139 0.056 Uiso 1 1 calc R . .
H1C H 0.3279 0.6844 0.5059 0.056 Uiso 1 1 calc R . .
H1D H 0.3544 0.7506 0.4075 0.056 Uiso 1 1 calc R . .
Zn2 Zn 0.07971(6) 1.00244(4) 0.67427(4) 0.0261(2) Uani 1 1 d . . .
O2 O 0.1038(3) 1.1368(2) 0.5897(2) 0.0248(7) Uani 1 1 d . . .
C2 C 0.0400(7) 0.9968(4) 0.8087(4) 0.0434(14) Uani 1 1 d . . .
H2B H -0.0332 1.0523 0.8184 0.065 Uiso 1 1 calc R . .
H2C H 0.1211 1.0186 0.8509 0.065 Uiso 1 1 calc R . .
H2D H 0.0121 0.9166 0.8245 0.065 Uiso 1 1 calc R . .
O3 O 0.2894(3) 0.9261(3) 0.6506(2) 0.0286(8) Uani 1 1 d . . .
C3 C -0.1814(5) 0.7305(4) 0.5576(3) 0.0261(10) Uani 1 1 d . . .
O4 O 0.0348(3) 0.8784(2) 0.5704(2) 0.0249(7) Uani 1 1 d . . .
C4 C -0.0941(6) 0.6275(4) 0.5249(4) 0.0362(13) Uani 1 1 d . . .
H4A H -0.1313 0.5522 0.5451 0.054 Uiso 1 1 calc R . .
H4B H -0.0010 0.6362 0.5547 0.054 Uiso 1 1 calc R . .
H4C H -0.0946 0.6288 0.4542 0.054 Uiso 1 1 calc R . .
C5 C -0.1786(5) 0.7306(4) 0.6681(3) 0.0299(11) Uani 1 1 d . . .
H5A H -0.2222 0.6586 0.6892 0.045 Uiso 1 1 calc R . .
H5B H -0.2273 0.8000 0.6888 0.045 Uiso 1 1 calc R . .
H5C H -0.0846 0.7331 0.6970 0.045 Uiso 1 1 calc R . .
C6 C -0.3249(5) 0.7190(4) 0.5109(4) 0.0346(12) Uani 1 1 d . . .
H6A H -0.3651 0.6461 0.5333 0.052 Uiso 1 1 calc R . .
H6B H -0.3243 0.7164 0.4403 0.052 Uiso 1 1 calc R . .
H6C H -0.3782 0.7870 0.5289 0.052 Uiso 1 1 calc R . .
C11 C 0.3225(5) 0.8249(4) 0.7154(4) 0.0331(11) Uani 1 1 d . . .
H11A H 0.2865 0.7505 0.6855 0.040 Uiso 1 1 calc R . .
H11B H 0.2845 0.8361 0.7782 0.040 Uiso 1 1 calc R . .
C12 C 0.4733(5) 0.8227(4) 0.7289(4) 0.0396(13) Uani 1 1 d . . .
H12A H 0.5106 0.7763 0.6770 0.048 Uiso 1 1 calc R . .
H12B H 0.5063 0.7886 0.7926 0.048 Uiso 1 1 calc R . .
C13 C 0.5114(6) 0.9514(5) 0.7232(5) 0.0499(16) Uani 1 1 d . . .
H13A H 0.5108 0.9900 0.7872 0.060 Uiso 1 1 calc R . .
H13B H 0.6025 0.9602 0.7007 0.060 Uiso 1 1 calc R . .
C14 C 0.4071(6) 1.0032(4) 0.6525(5) 0.0453(16) Uani 1 1 d . . .
H14A H 0.3838 1.0841 0.6726 0.054 Uiso 1 1 calc R . .
H14B H 0.4403 1.0073 0.5875 0.054 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'
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
C1 Zn1 O1 131.3(2) . . ?
C1 Zn1 O4 127.8(2) . . ?
O1 Zn1 O4 98.17(13) . . ?
C1 Zn1 O3 111.92(17) . . ?
O1 Zn1 O3 91.91(12) . . ?
O4 Zn1 O3 76.06(12) . . ?
O2 P1 O1 114.11(17) 3_576 3_576 ?
O2 P1 O4 109.2(2) 3_576 . ?
O1 P1 O4 109.54(17) 3_576 . ?
O2 P1 C3 108.45(19) 3_576 . ?
O1 P1 C3 108.0(2) 3_576 . ?
O4 P1 C3 107.39(19) . . ?
P1 O1 Zn1 126.3(2) 3_576 . ?
C2 Zn2 O2 130.63(17) . . ?
C2 Zn2 O4 127.35(19) . . ?
O2 Zn2 O4 98.26(13) . . ?
C2 Zn2 O3 113.2(2) . . ?
O2 Zn2 O3 92.35(13) . . ?
O4 Zn2 O3 77.26(12) . . ?
P1 O2 Zn2 126.07(17) 3_576 . ?
C14 O3 C11 108.8(3) . . ?
C14 O3 Zn2 120.5(3) . . ?
C11 O3 Zn2 110.8(3) . . ?
C14 O3 Zn1 114.6(3) . . ?
C11 O3 Zn1 113.0(3) . . ?
Zn2 O3 Zn1 87.90(11) . . ?
C6 C3 C5 110.7(4) . . ?
C6 C3 C4 110.0(4) . . ?
C5 C3 C4 109.8(4) . . ?
C6 C3 P1 108.9(3) . . ?
C5 C3 P1 109.0(3) . . ?
C4 C3 P1 108.5(3) . . ?
P1 O4 Zn1 120.96(18) . . ?
P1 O4 Zn2 120.47(19) . . ?
Zn1 O4 Zn2 106.00(15) . . ?
O3 C11 C12 104.6(4) . . ?
C11 C12 C13 103.4(4) . . ?
C14 C13 C12 104.7(4) . . ?
O3 C14 C13 106.5(4) . . ?
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 C1 1.940(5) . ?
Zn1 O1 1.943(3) . ?
Zn1 O4 2.028(4) . ?
Zn1 O3 2.360(3) . ?
P1 O2 1.518(3) 3_576 ?
P1 O1 1.523(3) 3_576 ?
P1 O4 1.551(3) . ?
P1 C3 1.811(4) . ?
O1 P1 1.523(3) 3_576 ?
Zn2 C2 1.943(6) . ?
Zn2 O2 1.949(3) . ?
Zn2 O4 2.029(3) . ?
Zn2 O3 2.308(3) . ?
O2 P1 1.518(3) 3_576 ?
O3 C14 1.457(6) . ?
O3 C11 1.471(5) . ?
C3 C6 1.512(7) . ?
C3 C5 1.529(6) . ?
C3 C4 1.547(7) . ?
C11 C12 1.492(7) . ?
C12 C13 1.509(7) . ?
C13 C14 1.476(7) . ?
