#------------------------------------------------------------------------------
#$Date: 2020-04-01 04:55:12 +0300 (Wed, 01 Apr 2020) $
#$Revision: 249893 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/02/7240230.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_7240230
loop_
_publ_author_name
'Goldman, Anna'
'Gil-Hernández, Beatriz'
'Millan, Simon'
'Gökpinar, Serkan'
'Heering, Christian'
'Boldog, Ishtvan'
'Janiak, Christoph'
_publ_section_title
;
 Flexible bifunctional monoethylphosphonate/carboxylates of Zn(II) and
 Co(II) reinforced with DABCO co-ligand: paradigmatic structural
 organization with pcu topology
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00275E
_journal_year                    2020
_chemical_formula_moiety         'C8 H7 O5.50 P1.25 Zn, C H2'
_chemical_formula_sum            'C9 H9 O5.5 P1.25 Zn'
_chemical_formula_weight         309.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4445(11)
_cell_length_b                   21.4445(11)
_cell_length_c                   9.3118(5)
_cell_measurement_reflns_used    16531
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      1.75
_cell_volume                     4282.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_molecular_graphics    'DIAMOND 4.5 (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.065
_diffrn_reflns_theta_min         1.343
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.959
_exptl_crystal_description       block
_exptl_crystal_F_000             1246
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylformamide'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.722
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1041P)²+8.4314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1636
_reflns_number_total             2112
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00275e2.cif
_cod_data_source_block           Zn_BCP_Et
_cod_original_cell_volume        4282.2(5)
_cod_original_formula_sum        'C9 H9 O5.50 P1.25 Zn'
_cod_database_code               7240230
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.976
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.500000 0.500000 0.33857(7) 0.0240(2) Uani 1 8 d S T P . .
Zn2 Zn 0.500000 1.000000 0.250000 0.0288(2) Uani 1 8 d S T P . .
O1 O 0.500000 0.92634(14) 0.3645(4) 0.0676(11) Uani 1 2 d S T P . .
P1 P 0.52771(13) 0.90154(9) 0.500000 0.0472(5) Uani 0.5 2 d S T P . .
O11 O 0.5987(5) 0.9153(5) 0.500000 0.097(3) Uiso 0.5 2 d DS U P . .
C11 C 0.6486(10) 0.8942(12) 0.427(2) 0.118(8) Uani 0.25 1 d D U P . .
H11A H 0.646517 0.906695 0.326786 0.141 Uiso 0.25 1 calc R U P . .
H11B H 0.651209 0.849116 0.431847 0.141 Uiso 0.25 1 calc R U P . .
C12 C 0.7033(14) 0.9239(18) 0.500000 0.256(18) Uani 0.5 2 d DS TU P . .
H12A H 0.741066 0.910947 0.453515 0.384 Uiso 0.25 1 calc R U P . .
H12B H 0.699532 0.968407 0.500000 0.384 Uiso 0.5 2 calc R U P . .
H12C H 0.704192 0.911225 0.598881 0.384 Uiso 0.25 1 calc R U P . .
C1 C 0.500000 0.8187(3) 0.500000 0.118(5) Uani 1 4 d S TU P . .
C2 C 0.500000 0.7860(2) 0.6270(6) 0.103(3) Uani 1 2 d S TU P . .
H2 H 0.500000 0.807538 0.713776 0.124 Uiso 1 2 calc R U P . .
C3 C 0.500000 0.7219(2) 0.6272(5) 0.083(2) Uani 1 2 d S TU P . .
H3 H 0.500000 0.700443 0.714001 0.099 Uiso 1 2 calc R U P . .
C4 C 0.500000 0.6893(3) 0.500000 0.0519(15) Uani 1 4 d S TU P . .
C5 C 0.500000 0.6195(2) 0.500000 0.0424(11) Uani 1 4 d S T P . .
O4 O 0.500000 0.59335(13) 0.3803(4) 0.0587(9) Uani 1 2 d S T P . .
O1X O 0.500000 0.500000 0.1326(6) 0.0458(13) Uani 1 8 d S T P . .
P1X P 0.500000 0.4640(3) 0.000000 0.073(3) Uani 0.25 4 d S T P . .
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
O1X Zn1 O4 100.99(10) . . ?
O1X Zn1 O4 100.99(10) . 4_565 ?
O4 Zn1 O4 87.92(4) . 4_565 ?
O1X Zn1 O4 100.99(10) . 3_655 ?
O4 Zn1 O4 87.92(4) . 3_655 ?
O4 Zn1 O4 158.03(19) 4_565 3_655 ?
O1X Zn1 O4 100.99(10) . 2_665 ?
O4 Zn1 O4 158.03(19) . 2_665 ?
O4 Zn1 O4 87.92(4) 4_565 2_665 ?
O4 Zn1 O4 87.92(4) 3_655 2_665 ?
O1X Zn1 Zn1 180.0 . 17_666 ?
O4 Zn1 Zn1 79.01(10) . 17_666 ?
O4 Zn1 Zn1 79.01(10) 4_565 17_666 ?
O4 Zn1 Zn1 79.01(10) 3_655 17_666 ?
O4 Zn1 Zn1 79.01(10) 2_665 17_666 ?
O1 Zn2 O1 108.23(10) 27_465 2_675 ?
O1 Zn2 O1 112.0(2) 27_465 28_655 ?
O1 Zn2 O1 108.23(11) 2_675 28_655 ?
O1 Zn2 O1 108.23(11) 27_465 . ?
O1 Zn2 O1 112.0(2) 2_675 . ?
O1 Zn2 O1 108.23(10) 28_655 . ?
P1 O1 P1 46.9(2) . 5_656 ?
P1 O1 Zn2 140.18(19) . . ?
P1 O1 Zn2 140.19(19) 5_656 . ?
P1 P1 O1 66.55(11) 5_656 18_556 ?
P1 P1 O1 66.55(11) 5_656 . ?
O1 P1 O1 115.4(2) 18_556 . ?
P1 P1 O11 169.0(4) 5_656 . ?
O1 P1 O11 108.8(2) 18_556 . ?
O1 P1 O11 108.8(2) . . ?
P1 P1 C1 71.50(11) 5_656 . ?
O1 P1 C1 102.21(15) 18_556 . ?
O1 P1 C1 102.21(15) . . ?
O11 P1 C1 119.5(4) . . ?
C11 O11 C11 61(2) 18_556 . ?
C11 O11 P1 135.7(13) 18_556 . ?
C11 O11 P1 135.7(13) . . ?
O11 C11 C12 104(2) . . ?
C2 C1 C2 118.7(6) 18_556 . ?
C2 C1 P1 118.9(3) 18_556 5_656 ?
C2 C1 P1 118.9(3) . 5_656 ?
C2 C1 P1 118.9(3) 18_556 . ?
C2 C1 P1 118.9(3) . . ?
C1 C2 C3 120.7(5) . . ?
C2 C3 C4 120.5(5) . . ?
C3 C4 C3 118.8(5) 18_556 . ?
C3 C4 C5 120.6(3) 18_556 . ?
C3 C4 C5 120.6(3) . . ?
O4 C5 O4 126.6(5) 18_556 . ?
O4 C5 C4 116.7(2) 18_556 . ?
O4 C5 C4 116.7(2) . . ?
C5 O4 Zn1 127.7(3) . . ?
P1X O1X P1X 64.1(5) 19_565 3_655 ?
P1X O1X P1X 64.1(5) . 17_665 ?
P1X O1X Zn1 148.0(3) . . ?
P1X O1X Zn1 148.0(3) 19_565 . ?
P1X O1X Zn1 148.0(3) 3_655 . ?
P1X O1X Zn1 148.0(3) 17_665 . ?
P1X P1X P1X 90.002(1) 3_655 19_565 ?
P1X P1X O1X 67.97(17) 3_655 . ?
P1X P1X O1X 67.97(17) 19_565 . ?
P1X P1X O1X 67.97(17) 3_655 17_665 ?
P1X P1X O1X 67.97(17) 19_565 17_665 ?
O1X P1X O1X 115.9(5) . 17_665 ?
P1X P1X P1X 45.001(1) 3_655 17_665 ?
P1X P1X P1X 45.001(1) 19_565 17_665 ?
O1X P1X P1X 58.0(3) . 17_665 ?
O1X P1X P1X 58.0(3) 17_665 17_665 ?
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 O1X 1.918(5) . ?
Zn1 O4 2.039(3) . ?
Zn1 O4 2.039(3) 4_565 ?
Zn1 O4 2.039(3) 3_655 ?
Zn1 O4 2.039(3) 2_665 ?
Zn1 Zn1 3.0064(13) 17_666 ?
Zn2 O1 1.906(3) 27_465 ?
Zn2 O1 1.906(3) 2_675 ?
Zn2 O1 1.906(3) 28_655 ?
Zn2 O1 1.906(3) . ?
O1 P1 1.493(3) . ?
O1 P1 1.493(3) 5_656 ?
P1 P1 1.188(5) 5_656 ?
P1 O11 1.552(11) . ?
P1 C1 1.873(7) . ?
O11 C11 1.347(16) 18_556 ?
O11 C11 1.347(16) . ?
C11 C12 1.497(18) . ?
C1 C2 1.375(6) 18_556 ?
C1 C2 1.375(6) . ?
C2 C3 1.375(6) . ?
C3 C4 1.376(6) . ?
C4 C5 1.497(7) . ?
C5 O4 1.247(4) 18_556 ?
C5 O4 1.247(4) . ?
O1X P1X 1.456(6) . ?
O1X P1X 1.456(6) 19_565 ?
O1X P1X 1.456(6) 3_655 ?
O1X P1X 1.456(6) 17_665 ?
P1X P1X 1.093(10) 3_655 ?
P1X P1X 1.093(10) 19_565 ?
P1X P1X 1.545(14) 17_665 ?
