#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:00:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179166 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/27/4312790.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_4312790
loop_
_publ_author_name
'Bidyut Kumar Santra'
'Ben-Jie Liaw'
'Chiu-Mine Hung'
'C. W. Liu'
'Ju-Chun Wang'
_publ_section_title
;
 Syntheses, Solid-State Structures, and Solution Studies by VT 31P NMR of
 [Zn{Se2P(OEt)2}2]∞ and [Zn2{Se2P(OiPr)2}4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8866
_journal_page_last               8871
_journal_paper_doi               10.1021/ic034845y
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C8 H20 O4 P2 Se4 Zn'
_chemical_formula_weight         623.39
_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                 105.272(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.558(3)
_cell_length_b                   19.803(7)
_cell_length_c                   11.901(4)
_cell_measurement_reflns_used    977
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.83
_cell_volume                     1945.7(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5906
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    8.913
_exptl_absorpt_correction_T_max  0.9224
_exptl_absorpt_correction_T_min  0.4042
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0677P)²+11.5101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                2426
_reflns_number_total             3307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034845ysi20030718_044519_1.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 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_original_cell_volume        1945.6(11)
_cod_database_code               4312790
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 0.79435(14) 0.33287(6) 0.63532(9) 0.0427(3) Uani 1 1 d . . .
Se1 Se 1.25903(12) 0.16592(6) 0.92268(8) 0.0445(3) Uani 1 1 d . . .
Se2 Se 1.03676(13) 0.26112(6) 0.68791(8) 0.0508(3) Uani 1 1 d . . .
Se3 Se 0.82077(16) 0.44935(6) 0.72257(12) 0.0662(4) Uani 1 1 d . . .
Se4 Se 0.55061(13) 0.31472(6) 0.70565(9) 0.0507(3) Uani 1 1 d . . .
P1 P 0.6183(4) 0.41248(16) 0.7808(2) 0.0539(7) Uani 1 1 d . . .
P6 P 1.0782(3) 0.24346(13) 0.87193(19) 0.0372(5) Uani 1 1 d . . .
O1 O 1.1232(8) 0.3093(4) 0.9474(6) 0.0469(16) Uani 1 1 d . . .
O2 O 0.9177(7) 0.2261(3) 0.9069(6) 0.0431(15) Uani 1 1 d . . .
O3 O 0.6459(11) 0.4138(5) 0.9167(6) 0.073(3) Uani 1 1 d . . .
O4 O 0.4708(11) 0.4636(5) 0.7544(7) 0.073(2) Uani 1 1 d . . .
C1 C 1.2547(15) 0.3523(6) 0.9338(11) 0.063(3) Uani 1 1 d . . .
H1A H 1.2322 0.3684 0.8542 0.076 Uiso 1 1 calc R . .
H1B H 1.3552 0.3269 0.9512 0.076 Uiso 1 1 calc R . .
C2 C 1.270(2) 0.4099(8) 1.0141(15) 0.100(5) Uani 1 1 d . . .
H2A H 1.3574 0.4384 1.0066 0.150 Uiso 1 1 calc R . .
H2B H 1.2916 0.3936 1.0927 0.150 Uiso 1 1 calc R . .
H2C H 1.1709 0.4353 0.9954 0.150 Uiso 1 1 calc R . .
C3 C 0.8322(15) 0.1657(6) 0.8681(12) 0.066(3) Uani 1 1 d . . .
H3A H 0.9016 0.1273 0.8969 0.080 Uiso 1 1 calc R . .
H3B H 0.8034 0.1643 0.7836 0.080 Uiso 1 1 calc R . .
C4 C 0.6838(16) 0.1607(7) 0.9086(13) 0.075(4) Uani 1 1 d . . .
H4A H 0.6294 0.1190 0.8818 0.112 Uiso 1 1 calc R . .
H4B H 0.6135 0.1979 0.8782 0.112 Uiso 1 1 calc R . .
H4C H 0.7121 0.1619 0.9921 0.112 Uiso 1 1 calc R . .
C5 C 0.761(2) 0.3707(11) 0.9908(11) 0.105(6) Uani 1 1 d . . .
H5A H 0.8564 0.3678 0.9610 0.126 Uiso 1 1 calc R . .
H5B H 0.7157 0.3258 0.9881 0.126 Uiso 1 1 calc R . .
C6 C 0.811(3) 0.3929(11) 1.1109(12) 0.125(7) Uani 1 1 d . . .
H6A H 0.8898 0.3619 1.1555 0.188 Uiso 1 1 calc R . .
H6B H 0.7188 0.3944 1.1422 0.188 Uiso 1 1 calc R . .
H6C H 0.8584 0.4371 1.1147 0.188 Uiso 1 1 calc R . .
C7 C 0.3814(17) 0.4805(8) 0.6370(12) 0.078(4) Uani 1 1 d . . .
H7A H 0.4077 0.4486 0.5827 0.094 Uiso 1 1 calc R . .
H7B H 0.4114 0.5253 0.6173 0.094 Uiso 1 1 calc R . .
C8 C 0.2086(17) 0.4782(8) 0.6272(13) 0.082(4) Uani 1 1 d . . .
H8A H 0.1497 0.4887 0.5488 0.122 Uiso 1 1 calc R . .
H8B H 0.1825 0.5106 0.6795 0.122 Uiso 1 1 calc R . .
H8C H 0.1794 0.4338 0.6471 0.122 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'
Se Se -0.0929 2.2259 '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
Se2 Zn1 Se1 97.70(5) . 4_565 ?
Se2 Zn1 Se4 124.16(6) . . ?
Se1 Zn1 Se4 117.55(6) 4_565 . ?
Se2 Zn1 Se3 116.58(6) . . ?
Se1 Zn1 Se3 112.82(6) 4_565 . ?
Se4 Zn1 Se3 89.18(6) . . ?
P6 Se1 Zn1 99.54(7) . 4_666 ?
P6 Se2 Zn1 104.78(8) . . ?
P1 Se3 Zn1 80.20(9) . . ?
P1 Se4 Zn1 81.42(9) . . ?
O3 P1 O4 95.1(5) . . ?
O3 P1 Se4 113.2(4) . . ?
O4 P1 Se4 112.4(4) . . ?
O3 P1 Se3 114.1(4) . . ?
O4 P1 Se3 112.7(4) . . ?
Se4 P1 Se3 108.83(13) . . ?
O1 P6 O2 97.4(4) . . ?
O1 P6 Se1 112.4(3) . . ?
O2 P6 Se1 112.5(3) . . ?
O1 P6 Se2 113.4(3) . . ?
O2 P6 Se2 112.5(3) . . ?
Se1 P6 Se2 108.38(11) . . ?
C1 O1 P6 120.2(7) . . ?
C3 O2 P6 120.7(7) . . ?
C5 O3 P1 121.3(8) . . ?
C7 O4 P1 122.0(8) . . ?
O1 C1 C2 108.7(11) . . ?
O2 C3 C4 111.5(11) . . ?
O3 C5 C6 114.0(15) . . ?
O4 C7 C8 109.8(11) . . ?
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 Se2 2.4557(16) . ?
Zn1 Se1 2.4684(16) 4_565 ?
Zn1 Se4 2.4700(17) . ?
Zn1 Se3 2.5150(18) . ?
Se1 P6 2.150(3) . ?
Se1 Zn1 2.4684(16) 4_666 ?
Se2 P6 2.153(2) . ?
Se3 P1 2.156(3) . ?
Se4 P1 2.147(3) . ?
P1 O3 1.572(8) . ?
P1 O4 1.584(9) . ?
P6 O1 1.572(7) . ?
P6 O2 1.575(7) . ?
O1 C1 1.454(14) . ?
O2 C3 1.414(13) . ?
O3 C5 1.423(17) . ?
O4 C7 1.445(14) . ?
C1 C2 1.471(17) . ?
C3 C4 1.475(17) . ?
C5 C6 1.449(19) . ?
C7 C8 1.453(19) . ?
