#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:40:48 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/91/7709175.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_7709175
loop_
_publ_author_name
'Passadis, Stamatis S.'
'Hadjithoma, Sofia'
'Papanikolaou, Michael G.'
'Keramidas, Anastasios D.'
'Miras, Haralampos N.'
'Kabanos, Themistoklis A.'
_publ_section_title
;
 Acid/base responsive assembly/dis-assembly of a family of zirconium(IV)
 clusters with a cyclic imide-dioxime ligand.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1806
_journal_page_last               1818
_journal_paper_doi               10.1039/d1dt03641f
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C10 H19.60 N6 O6 Zr, C H4 O, 2(Cl), H2 O '
_chemical_formula_sum            'C11 H25.6 Cl2 N6 O8 Zr'
_chemical_formula_weight         532.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9010(6)
_cell_length_b                   14.1221(5)
_cell_length_c                   17.6833(9)
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      30.5160
_cell_measurement_theta_min      2.6330
_cell_volume                     3970.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      174(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             2173
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3310
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0376P)²+2.9682P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2573
_reflns_number_total             3310
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03641f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7709175--7709176.cif.'
_cod_original_formula_sum        'C11 H25.60 Cl2 N6 O8 Zr'
_cod_database_code               7709175
_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   0.918
_shelx_estimated_absorpt_t_max   0.941
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
C1 C 0.2053(2) 0.5632(2) 0.2614(2) 0.0187(8) Uani 1 1 d . . . A 1
C5 C 0.3831(2) 0.2182(2) 0.4160(2) 0.0226(8) Uani 1 1 d . . . A 1
C6 C 0.3903(3) 0.1348(3) 0.4673(2) 0.0344(10) Uani 1 1 d . . . A 1
H6A H 0.450408 0.120958 0.476881 0.041 Uiso 1 1 calc R U . A 1
H6B H 0.364984 0.078660 0.442659 0.041 Uiso 1 1 calc R U . A 1
C7 C 0.3467(3) 0.1533(4) 0.5408(3) 0.0375(13) Uani 0.8 1 d . . P A 1
H7A H 0.341804 0.093017 0.569080 0.045 Uiso 0.8 1 calc R U P A 1
H7B H 0.381377 0.197106 0.571371 0.045 Uiso 0.8 1 calc R U P A 1
C8 C 0.2612(3) 0.1948(3) 0.5311(3) 0.0422(11) Uani 1 1 d . . . A 1
H8A H 0.239761 0.216651 0.580701 0.051 Uiso 1 1 calc R U . A 1
H8B H 0.222278 0.145797 0.511656 0.051 Uiso 1 1 calc R U . A 1
C9 C 0.2639(2) 0.2762(3) 0.4773(2) 0.0308(9) Uani 1 1 d . . . A 1
C15 C 0.1455(2) 0.6085(3) 0.2071(2) 0.0301(9) Uani 1 1 d . . . A 1
H15A H 0.167192 0.671310 0.191642 0.036 Uiso 1 1 calc R U . A 1
H15B H 0.090174 0.617837 0.231800 0.036 Uiso 1 1 calc R U . A 1
C16 C 0.1355(3) 0.5453(3) 0.1379(2) 0.0358(10) Uani 1 1 d . . . A 1
H16A H 0.189233 0.542155 0.109807 0.043 Uiso 1 1 calc R U . A 1
H16B H 0.092011 0.571749 0.103887 0.043 Uiso 1 1 calc R U . A 1
C17 C 0.1096(2) 0.4457(3) 0.1638(2) 0.0283(9) Uani 1 1 d . . . A 1
H17A H 0.052875 0.447754 0.186766 0.034 Uiso 1 1 calc R U . A 1
H17B H 0.107831 0.402402 0.119818 0.034 Uiso 1 1 calc R U . A 1
C18 C 0.1714(2) 0.4109(3) 0.2199(2) 0.0208(8) Uani 1 1 d . . . A 1
Cl1 Cl 0.61854(5) 0.13712(6) 0.35665(5) 0.0228(2) Uani 1 1 d . . . B 1
Cl2 Cl 0.53704(6) 0.34259(7) 0.51142(6) 0.0309(2) Uani 1 1 d . . . C 1
N1 N 0.2130(2) 0.3474(2) 0.4807(2) 0.0387(9) Uani 1 1 d . . . A 1
H1 H 0.171055 0.348254 0.513177 0.046 Uiso 1 1 calc R U . A 1
N2 N 0.43475(18) 0.2364(2) 0.36209(17) 0.0225(7) Uani 1 1 d . . . A 1
H2 H 0.477347 0.198247 0.353150 0.027 Uiso 1 1 calc R U . A 1
N3 N 0.32069(18) 0.2833(2) 0.42156(17) 0.0236(7) Uani 1 1 d . . . A 1
N4 N 0.25275(18) 0.61010(19) 0.30675(16) 0.0201(7) Uani 1 1 d . . . A 1
H4 H 0.250741 0.672366 0.307470 0.024 Uiso 1 1 calc R U . A 1
N5 N 0.21535(18) 0.4682(2) 0.26659(17) 0.0208(7) Uani 1 1 d . . . A 1
N6 N 0.19051(18) 0.3224(2) 0.22808(17) 0.0241(7) Uani 1 1 d . . . A 1
H6 H 0.166454 0.278590 0.200108 0.029 Uiso 1 1 calc R U . A 1
O29 O 0.5439(2) 0.1904(2) 0.18409(19) 0.0495(8) Uani 1 1 d D . . D 1
O2 O 0.2261(3) 0.4214(3) 0.4324(2) 0.0294(10) Uani 0.8 1 d . . P A 1
O11 O 0.42320(15) 0.31515(17) 0.31879(14) 0.0229(6) Uani 1 1 d . . . A 1
O21 O 0.30591(15) 0.56312(17) 0.35347(14) 0.0251(6) Uani 1 1 d . . . A 1
O23 O 0.24922(16) 0.29900(16) 0.28151(15) 0.0272(6) Uani 1 1 d . . . A 1
O24 O 0.41111(18) 0.46298(18) 0.42479(16) 0.0337(7) Uani 1 1 d D . . A 1
O25 O 0.39004(18) 0.45651(19) 0.24276(16) 0.0328(7) Uani 1 1 d D . . A 1
Zr1 Zr 0.31688(2) 0.40896(2) 0.34318(2) 0.01840(11) Uani 1 1 d D . . A 1
O2B O 0.2016(10) 0.4044(13) 0.4135(10) 0.019(5) Uiso 0.2 1 d . . P E 2
C7B C 0.3117(12) 0.1156(13) 0.5092(11) 0.020(4) Uiso 0.2 1 d . . P F 2
O28B O 0.5139(5) 0.3752(5) 0.1799(3) 0.0675(17) Uani 0.7 1 d D . P G 2
H28B H 0.524971 0.317067 0.182079 0.101 Uiso 0.7 1 calc R U P G 2
C28B C 0.5345(5) 0.4090(6) 0.1102(5) 0.054(2) Uani 0.7 1 d D . P G 2
H28A H 0.494962 0.458991 0.095824 0.081 Uiso 0.7 1 calc R U P G 2
H28C H 0.531789 0.357398 0.073219 0.081 Uiso 0.7 1 calc R U P G 2
H28D H 0.591728 0.434793 0.111494 0.081 Uiso 0.7 1 calc R U P G 2
C28 C 0.5485(11) 0.3899(18) 0.1402(16) 0.054(7) Uiso 0.3 1 d D . P H 3
H28E H 0.546166 0.458858 0.146082 0.081 Uiso 0.3 1 calc R U P H 3
H28F H 0.566449 0.374303 0.088656 0.081 Uiso 0.3 1 calc R U P H 3
H28G H 0.588637 0.363444 0.176502 0.081 Uiso 0.3 1 calc R U P H 3
O28 O 0.4680(7) 0.3512(9) 0.1536(7) 0.044(3) Uani 0.3 1 d D . P H 3
H28 H 0.472333 0.292670 0.161148 0.065 Uiso 0.3 1 calc R U P H 3
H24A H 0.445(2) 0.431(2) 0.452(2) 0.065 Uiso 1 1 d D U . I 1
H24B H 0.418(3) 0.5214(16) 0.439(2) 0.065 Uiso 1 1 d D U . J 1
H25A H 0.427(3) 0.425(2) 0.218(2) 0.065 Uiso 1 1 d D U . K 1
H25B H 0.384(3) 0.508(2) 0.218(2) 0.065 Uiso 1 1 d D U . L 1
H29B H 0.581(2) 0.158(3) 0.211(2) 0.065 Uiso 1 1 d D U . . .
H29A H 0.546(3) 0.168(3) 0.1369(14) 0.065 Uiso 1 1 d D U . . .
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'
Cl Cl 0.1484 0.1585 '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'
Zr Zr -2.9673 0.5597 '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
N4 C1 N5 113.6(3) . . ?
N4 C1 C15 123.6(3) . . ?
N5 C1 C15 122.9(3) . . ?
N2 C5 N3 112.7(3) . . ?
N2 C5 C6 124.1(3) . . ?
N3 C5 C6 123.2(3) . . ?
C5 C6 C7 110.8(4) . . ?
C8 C7 C6 113.1(4) . . ?
C7 C8 C9 110.5(4) . . ?
N1 C9 N3 113.4(3) . . ?
N1 C9 C8 123.5(4) . . ?
N3 C9 C8 123.1(3) . . ?
C1 C15 C16 109.3(3) . . ?
C15 C16 C17 109.0(3) . . ?
C18 C17 C16 109.1(3) . . ?
N6 C18 N5 112.9(3) . . ?
N6 C18 C17 123.5(3) . . ?
N5 C18 C17 123.6(3) . . ?
C9 N1 O2 118.1(4) . . ?
C5 N2 O11 119.6(3) . . ?
C9 N3 C5 119.7(3) . . ?
C9 N3 Zr1 119.6(2) . . ?
C5 N3 Zr1 120.6(2) . . ?
C1 N4 O21 119.6(3) . . ?
C18 N5 C1 119.4(3) . . ?
C18 N5 Zr1 120.8(2) . . ?
C1 N5 Zr1 119.3(2) . . ?
C18 N6 O23 118.1(3) . . ?
N1 O2 Zr1 120.0(3) . . ?
N2 O11 Zr1 119.14(19) . . ?
N4 O21 Zr1 119.03(19) . . ?
N6 O23 Zr1 120.62(18) . . ?
O2 Zr1 O23 95.38(15) . . ?
O2 Zr1 O11 135.52(12) . . ?
O23 Zr1 O11 81.47(9) . . ?
O2 Zr1 O21 78.71(13) . . ?
O23 Zr1 O21 135.19(9) . . ?
O11 Zr1 O21 132.72(9) . . ?
O2 Zr1 O24 87.03(15) . . ?
O23 Zr1 O24 154.72(9) . . ?
O11 Zr1 O24 79.32(10) . . ?
O21 Zr1 O24 69.98(9) . . ?
O2 Zr1 O25 155.96(12) . . ?
O23 Zr1 O25 94.23(11) . . ?
O11 Zr1 O25 67.80(9) . . ?
O21 Zr1 O25 78.94(10) . . ?
O24 Zr1 O25 93.57(11) . . ?
O2 Zr1 N3 68.29(13) . . ?
O23 Zr1 N3 76.12(10) . . ?
O11 Zr1 N3 67.92(10) . . ?
O21 Zr1 N3 137.19(10) . . ?
O24 Zr1 N3 81.50(10) . . ?
O25 Zr1 N3 135.59(10) . . ?
O2 Zr1 N5 85.97(14) . . ?
O23 Zr1 N5 67.23(9) . . ?
O11 Zr1 N5 130.93(10) . . ?
O21 Zr1 N5 68.05(10) . . ?
O24 Zr1 N5 138.02(10) . . ?
O25 Zr1 N5 77.54(10) . . ?
N3 Zr1 N5 132.65(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
C1 N4 1.285(4) . ?
C1 N5 1.353(4) . ?
C1 C15 1.496(5) . ?
C5 N2 1.285(5) . ?
C5 N3 1.356(4) . ?
C5 C6 1.492(5) . ?
C6 C7 1.496(7) . ?
C7 C8 1.490(7) . ?
C8 C9 1.493(5) . ?
C9 N1 1.293(5) . ?
C9 N3 1.341(5) . ?
C15 C16 1.523(6) . ?
C16 C17 1.535(5) . ?
C17 C18 1.480(5) . ?
C18 N6 1.293(4) . ?
C18 N5 1.352(4) . ?
N1 O2 1.365(5) . ?
N2 O11 1.362(4) . ?
N3 Zr1 2.252(3) . ?
N4 O21 1.355(4) . ?
N5 Zr1 2.267(3) . ?
N6 O23 1.369(4) . ?
O2 Zr1 2.146(4) . ?
O11 Zr1 2.191(2) . ?
O21 Zr1 2.192(2) . ?
O23 Zr1 2.181(2) . ?
O24 Zr1 2.216(3) . ?
O25 Zr1 2.227(3) . ?
O28B C28B 1.361(9) . ?
C28 O28 1.412(17) . ?
