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#$Date: 2022-05-05 23:49:55 +0300 (Thu, 05 May 2022) $
#$Revision: 275044 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/13/7061364.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_7061364
loop_
_publ_author_name
'Panja, Anangamohan'
'Jagličić, Zvonko'
'Herchel, Radovan'
'Brandão, Paula'
'Pramanik, Kuheli'
'Jana, Narayan Ch.'
_publ_section_title
;
 The first exploration of coordination chemistry using a methyl
 substituted o-vanillin based ligand: an example starting with Dy4/Zn2Dy2
 systems displaying slow relaxation of magnetization
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5627
_journal_page_last               5637
_journal_paper_doi               10.1039/D1NJ05717K
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C9 H10 O3'
_chemical_formula_weight         166.17
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-31 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.8905(3)
_cell_length_b                   10.3802(3)
_cell_length_c                   17.6535(5)
_cell_measurement_reflns_used    534
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.92
_cell_volume                     1629.16(9)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Mercury (Macrae et al 2008)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18411
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.149
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker, 2014)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       Block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0423
_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)+(0.0604P)²+0.5477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1728
_reflns_number_total             2188
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj05717k2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7061362--7061365.cif.'
_cod_database_code               7061364
_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   0.964
_shelx_estimated_absorpt_t_max   0.980
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
O2 O 0.39831(10) 0.30910(8) 0.71248(5) 0.0256(2) Uani 1 1 d . . . . .
O1 O 0.57074(10) 0.45878(9) 0.62869(5) 0.0268(2) Uani 1 1 d . . . . .
O3 O 0.58823(11) 0.66348(10) 0.54021(6) 0.0362(3) Uani 1 1 d . . . . .
C2 C 0.32581(13) 0.39917(10) 0.66931(6) 0.0204(2) Uani 1 1 d . . . . .
C1 C 0.42002(13) 0.47913(11) 0.62597(6) 0.0204(3) Uani 1 1 d . . . . .
C6 C 0.35470(14) 0.57670(11) 0.58197(6) 0.0230(3) Uani 1 1 d . . . . .
C5 C 0.19779(15) 0.59162(12) 0.57942(7) 0.0260(3) Uani 1 1 d . . . . .
H4 H 0.155087 0.657387 0.548792 0.031 Uiso 1 1 calc R U . . .
C4 C 0.10511(14) 0.51198(13) 0.62084(7) 0.0256(3) Uani 1 1 d . . . . .
C3 C 0.17144(13) 0.41627(11) 0.66646(7) 0.0230(3) Uani 1 1 d . . . . .
H6 H 0.108608 0.362001 0.696062 0.028 Uiso 1 1 calc R U . . .
C7 C 0.30563(16) 0.23131(12) 0.76086(7) 0.0294(3) Uani 1 1 d . . . . .
H7A H 0.249571 0.286996 0.795678 0.044 Uiso 1 1 calc R U . . .
H7B H 0.369209 0.172211 0.789997 0.044 Uiso 1 1 calc R U . . .
H7C H 0.234839 0.181609 0.729930 0.044 Uiso 1 1 calc R U . . .
C9 C 0.44960(17) 0.66635(12) 0.54026(7) 0.0302(3) Uani 1 1 d . . . . .
H8 H 0.401502 0.731362 0.511143 0.036 Uiso 1 1 calc R U . . .
C8 C -0.06357(16) 0.52708(17) 0.61981(9) 0.0383(4) Uani 1 1 d . . . . .
H8A H -0.089499 0.613882 0.602317 0.057 Uiso 1 1 calc R U . . .
H8B H -0.103343 0.513973 0.671005 0.057 Uiso 1 1 calc R U . . .
H8C H -0.107479 0.463191 0.585437 0.057 Uiso 1 1 calc R U . . .
H1 H 0.608(2) 0.5206(18) 0.5976(10) 0.045(5) Uiso 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'
O O 0.0106 0.0060 '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
C2 O2 C7 116.46(9) . . ?
C1 O1 H1 103.1(11) . . ?
O2 C2 C3 125.10(11) . . ?
O2 C2 C1 115.22(10) . . ?
C3 C2 C1 119.67(11) . . ?
O1 C1 C6 122.74(11) . . ?
O1 C1 C2 118.49(10) . . ?
C6 C1 C2 118.77(11) . . ?
C1 C6 C5 120.58(11) . . ?
C1 C6 C9 120.12(12) . . ?
C5 C6 C9 119.27(11) . . ?
C4 C5 C6 120.74(11) . . ?
C4 C5 H4 119.6 . . ?
C6 C5 H4 119.6 . . ?
C5 C4 C3 118.46(12) . . ?
C5 C4 C8 121.75(12) . . ?
C3 C4 C8 119.78(12) . . ?
C2 C3 C4 121.75(11) . . ?
C2 C3 H6 119.1 . . ?
C4 C3 H6 119.1 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C9 C6 124.35(12) . . ?
O3 C9 H8 117.8 . . ?
C6 C9 H8 117.8 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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
O2 C2 1.3677(14) . ?
O2 C7 1.4353(15) . ?
O1 C1 1.3574(14) . ?
O1 H1 0.907(19) . ?
O3 C9 1.2328(17) . ?
C2 C3 1.3848(16) . ?
C2 C1 1.4057(16) . ?
C1 C6 1.4022(16) . ?
C6 C5 1.4043(18) . ?
C6 C9 1.4560(17) . ?
C5 C4 1.3773(18) . ?
C5 H4 0.9500 . ?
C4 C3 1.4083(17) . ?
C4 C8 1.5078(18) . ?
C3 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H8 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
