#------------------------------------------------------------------------------
#$Date: 2019-11-24 11:41:37 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/53/7125373.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_7125373
loop_
_publ_author_name
'Sharma, Kamna'
'Gupta, Sandeep K.'
'Borah, Aditya'
'Murugavel, Ramaswamy'
_publ_section_title
;
 Hitherto unknown eight-connected frameworks formed from
 A₄B₄O₁₂ metal organophosphate
 heterocubanes.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7994
_journal_page_last               7997
_journal_paper_doi               10.1039/c9cc01893j
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C14 H20 N O5 P Zn, 2(H2 O), O [+ solvent]'
_chemical_formula_sum            'C14 H24 N O8 P Zn'
_chemical_formula_weight         430.68
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-05 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7211(2)
_cell_length_b                   16.7211(2)
_cell_length_c                   15.5352(4)
_cell_measurement_reflns_used    24287
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.7650
_cell_measurement_theta_min      1.8490
_cell_volume                     4343.57(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49457
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0645P)²+2.9211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3619
_reflns_number_total             3810
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc01893j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_original_cell_volume        4343.57(15)
_cod_database_code               7125373
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'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'
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
Zn1 Zn -0.61770(3) -0.44358(3) -0.59579(4) 0.0264(2) Uani 1 1 d . .
P1 P -0.55004(8) -0.62907(8) -0.60595(9) 0.0277(3) Uani 1 1 d . .
O1 O -0.5877(2) -0.6915(2) -0.6730(3) 0.0302(9) Uani 1 1 d . .
O5 O -0.9111(3) -0.7892(2) -0.8348(3) 0.0373(10) Uani 1 1 d . .
O4 O -0.4616(2) -0.6340(3) -0.6268(3) 0.0459(12) Uani 1 1 d . .
O3 O -0.5679(3) -0.6605(3) -0.5179(3) 0.0469(12) Uani 1 1 d . .
O2 O -0.5865(2) -0.5496(2) -0.6236(3) 0.0367(10) Uani 1 1 d . .
N1 N -0.8892(3) -0.6590(3) -0.8213(5) 0.0490(15) Uani 1 1 d . .
H1 H -0.9076 -0.6115 -0.8288 0.059 Uiso 1 1 calc R U
C5 C -0.8029(4) -0.7136(3) -0.7075(5) 0.0385(15) Uani 1 1 d . .
H5 H -0.8469 -0.7393 -0.6835 0.046 Uiso 1 1 calc R U
C6 C -0.7288(3) -0.7219(3) -0.6695(4) 0.0334(13) Uani 1 1 d . .
C3 C -0.7499(4) -0.6273(4) -0.8166(5) 0.0403(15) Uani 1 1 d . .
H3 H -0.7580 -0.5954 -0.8649 0.048 Uiso 1 1 calc R U
C2 C -0.6731(3) -0.6333(4) -0.7812(4) 0.0352(14) Uani 1 1 d . .
C10 C -0.7184(4) -0.7707(4) -0.5891(5) 0.0435(15) Uani 1 1 d . .
H10 H -0.6610 -0.7773 -0.5786 0.052 Uiso 1 1 calc R U
C1 C -0.6647(3) -0.6812(3) -0.7078(4) 0.0291(12) Uani 1 1 d . .
C4 C -0.8129(3) -0.6673(4) -0.7814(5) 0.0393(15) Uani 1 1 d . .
C13 C -0.9332(4) -0.7199(3) -0.8473(4) 0.0355(14) Uani 1 1 d . .
C11 C -0.7552(5) -0.7250(5) -0.5118(5) 0.0538(19) Uani 1 1 d . .
H11A H -0.7367 -0.6706 -0.5122 0.081 Uiso 1 1 calc R U
H11B H -0.7391 -0.7503 -0.4590 0.081 Uiso 1 1 calc R U
H11C H -0.8124 -0.7258 -0.5162 0.081 Uiso 1 1 calc R U
C7 C -0.6022(4) -0.5940(4) -0.8250(4) 0.0413(15) Uani 1 1 d . .
H7 H -0.5605 -0.5871 -0.7813 0.050 Uiso 1 1 calc R U
C8 C -0.6218(5) -0.5117(5) -0.8604(6) 0.070(2) Uani 1 1 d . .
H8A H -0.6582 -0.5169 -0.9079 0.104 Uiso 1 1 calc R U
H8B H -0.5735 -0.4863 -0.8796 0.104 Uiso 1 1 calc R U
H8C H -0.6461 -0.4799 -0.8161 0.104 Uiso 1 1 calc R U
C14 C -1.0113(3) -0.7024(4) -0.8937(6) 0.0471(18) Uani 1 1 d . .
H14A H -1.0045 -0.7110 -0.9543 0.071 Uiso 1 1 calc R U
H14B H -1.0265 -0.6478 -0.8836 0.071 Uiso 1 1 calc R U
H14C H -1.0524 -0.7373 -0.8723 0.071 Uiso 1 1 calc R U
C12 C -0.7564(5) -0.8535(4) -0.5946(6) 0.064(2) Uani 1 1 d . .
H12A H -0.8121 -0.8483 -0.6087 0.095 Uiso 1 1 calc R U
H12B H -0.7510 -0.8802 -0.5402 0.095 Uiso 1 1 calc R U
H12C H -0.7300 -0.8842 -0.6385 0.095 Uiso 1 1 calc R U
C9 C -0.5683(5) -0.6496(7) -0.8948(7) 0.086(3) Uani 1 1 d . .
H9A H -0.5503 -0.6985 -0.8688 0.129 Uiso 1 1 calc R U
H9B H -0.5242 -0.6238 -0.9230 0.129 Uiso 1 1 calc R U
H9C H -0.6092 -0.6613 -0.9363 0.129 Uiso 1 1 calc R U
O6 O -0.7231(3) -0.8885(3) -0.8268(4) 0.0708(16) Uani 1 1 d G .
H6A H -0.7308 -0.8391 -0.8369 0.106 Uiso 1 1 d G U
H6B H -0.7687 -0.9100 -0.8346 0.106 Uiso 1 1 d G U
O7 O -0.6101(4) -0.9726(5) -0.7227(5) 0.109(3) Uani 1 1 d G .
H7A H -0.6431 -0.9985 -0.7536 0.164 Uiso 1 1 d G U
H7B H -0.6123 -0.9251 -0.7419 0.164 Uiso 1 1 d G U
O8 O -0.5709(6) -0.8852(8) -0.9247(7) 0.153(4) 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
O2 Zn1 O3 113.9(2) . 3_544
O2 Zn1 O4 112.64(19) . 2_445
O3 Zn1 O4 115.0(2) 3_544 2_445
O2 Zn1 O5 110.52(18) . 8_353
O3 Zn1 O5 100.46(18) 3_544 8_353
O4 Zn1 O5 102.88(17) 2_445 8_353
O2 P1 O3 113.6(3) . .
O2 P1 O4 114.2(3) . .
O3 P1 O4 111.8(3) . .
O2 P1 O1 107.5(2) . .
O3 P1 O1 106.7(2) . .
O4 P1 O1 102.1(2) . .
C1 O1 P1 122.0(3) . .
C13 O5 Zn1 125.1(4) . 7_433
P1 O4 Zn1 125.7(3) . 2_445
P1 O3 Zn1 133.8(3) . 4_454
P1 O2 Zn1 154.9(3) . .
C13 N1 C4 123.8(5) . .
C6 C5 C4 121.1(6) . .
C5 C6 C1 117.1(6) . .
C5 C6 C10 121.0(6) . .
C1 C6 C10 121.8(5) . .
C4 C3 C2 121.0(7) . .
C1 C2 C3 117.0(6) . .
C1 C2 C7 122.4(5) . .
C3 C2 C7 120.6(6) . .
C6 C10 C12 113.5(6) . .
C6 C10 C11 109.3(5) . .
C12 C10 C11 109.0(6) . .
C2 C1 C6 123.1(5) . .
C2 C1 O1 118.4(5) . .
C6 C1 O1 118.5(5) . .
C3 C4 C5 120.7(6) . .
C3 C4 N1 118.0(7) . .
C5 C4 N1 121.3(6) . .
O5 C13 N1 120.7(6) . .
O5 C13 C14 120.9(5) . .
N1 C13 C14 118.4(5) . .
C2 C7 C8 112.8(6) . .
C2 C7 C9 110.1(6) . .
C8 C7 C9 111.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.898(4) .
Zn1 O3 1.916(4) 3_544
Zn1 O4 1.917(4) 2_445
Zn1 O5 1.970(4) 8_353
P1 O2 1.487(4) .
P1 O3 1.495(5) .
P1 O4 1.516(4) .
P1 O1 1.603(4) .
O1 C1 1.406(7) .
O5 C13 1.230(7) .
O5 Zn1 1.970(4) 7_433
O4 Zn1 1.917(4) 2_445
O3 Zn1 1.916(4) 4_454
N1 C13 1.320(8) .
N1 C4 1.424(8) .
C5 C6 1.380(9) .
C5 C4 1.394(10) .
C6 C1 1.404(8) .
C6 C10 1.501(9) .
C3 C4 1.364(9) .
C3 C2 1.402(9) .
C2 C1 1.400(9) .
C2 C7 1.516(9) .
C10 C12 1.526(9) .
C10 C11 1.552(10) .
C13 C14 1.521(9) .
C7 C8 1.518(11) .
C7 C9 1.537(11) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14A O3 0.96 2.66 3.277(9) 122.7 6_334
O6 H6B O4 0.85 1.94 2.779(7) 169.9 8_343
O7 H7B O6 0.85 2.36 2.858 118.3 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 P1 O1 C1 -27.9(5) . .
O3 P1 O1 C1 94.2(5) . .
O4 P1 O1 C1 -148.4(4) . .
O2 P1 O4 Zn1 46.1(5) . 2_445
O3 P1 O4 Zn1 -84.6(4) . 2_445
O1 P1 O4 Zn1 161.7(3) . 2_445
O2 P1 O3 Zn1 -52.8(5) . 4_454
O4 P1 O3 Zn1 78.2(5) . 4_454
O1 P1 O3 Zn1 -171.0(4) . 4_454
O3 P1 O2 Zn1 40.2(8) . .
O4 P1 O2 Zn1 -89.6(7) . .
O1 P1 O2 Zn1 158.0(6) . .
O3 Zn1 O2 P1 -40.6(7) 3_544 .
O4 Zn1 O2 P1 92.7(7) 2_445 .
O5 Zn1 O2 P1 -152.8(6) 8_353 .
C4 C5 C6 C1 0.7(9) . .
C4 C5 C6 C10 179.0(6) . .
C4 C3 C2 C1 -0.9(9) . .
C4 C3 C2 C7 175.0(6) . .
C5 C6 C10 C12 49.4(9) . .
C1 C6 C10 C12 -132.4(7) . .
C5 C6 C10 C11 -72.5(7) . .
C1 C6 C10 C11 105.8(7) . .
C3 C2 C1 C6 -0.2(8) . .
C7 C2 C1 C6 -176.0(5) . .
C3 C2 C1 O1 177.1(5) . .
C7 C2 C1 O1 1.3(8) . .
C5 C6 C1 C2 0.3(8) . .
C10 C6 C1 C2 -178.0(6) . .
C5 C6 C1 O1 -177.0(5) . .
C10 C6 C1 O1 4.7(8) . .
P1 O1 C1 C2 85.8(6) . .
P1 O1 C1 C6 -96.8(5) . .
C2 C3 C4 C5 1.9(9) . .
C2 C3 C4 N1 -179.4(6) . .
C6 C5 C4 C3 -1.8(9) . .
C6 C5 C4 N1 179.6(6) . .
C13 N1 C4 C3 125.5(7) . .
C13 N1 C4 C5 -55.9(10) . .
Zn1 O5 C13 N1 -155.0(5) 7_433 .
Zn1 O5 C13 C14 24.5(9) 7_433 .
C4 N1 C13 O5 3.1(11) . .
C4 N1 C13 C14 -176.5(7) . .
C1 C2 C7 C8 -143.7(7) . .
C3 C2 C7 C8 40.6(8) . .
C1 C2 C7 C9 90.6(8) . .
C3 C2 C7 C9 -85.1(9) . .
