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#$Date: 2021-09-06 13:23:49 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268647 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/31/7243131.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_7243131
loop_
_publ_author_name
'Mylonas-Margaritis, Ioannis'
'Mayans, Júlia'
'Tong, Wenming'
'Farràs, Pau'
'Escuer, Albert'
'McArdle, Patrick'
'Papatriantafyllopoulou, Constantina'
_publ_section_title
;
 Synthesis and characterization of new coordination compounds by the use
 of 2-pyridinemethanol and di- or tricarboxylic acids
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              5489
_journal_page_last               5497
_journal_paper_doi               10.1039/D1CE00659B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C14.5 H11.5 N1.5 Ni0.75 O6.62'
_chemical_formula_weight         356.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-27 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.471(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3588(7)
_cell_length_b                   30.0187(10)
_cell_length_c                   12.2991(8)
_cell_measurement_reflns_used    4255
_cell_measurement_temperature    297.1(8)
_cell_measurement_theta_max      28.5370
_cell_measurement_theta_min      3.7150
_cell_volume                     3720.8(4)
_computing_cell_refinement       'crysalispro 1.171.40.14e (rigaku od, 2018)'
_computing_data_collection       'crysalispro 1.171.40.14e (rigaku od, 2018)'
_computing_data_reduction        'crysalispro 1.171.40.14e (rigaku od, 2018)'
_computing_molecular_graphics
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297.1(8)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.801
_diffrn_measured_fraction_theta_max 0.707
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.801
_diffrn_reflns_Laue_measured_fraction_max 0.707
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9849
_diffrn_reflns_point_group_measured_fraction_full 0.801
_diffrn_reflns_point_group_measured_fraction_max 0.707
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.091
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'fine-focus sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
crysalispro 1.171.40.14e (rigaku oxford diffraction, 2018) 
empirical absorption correction using spherical harmonics, 
 implemented in scale3 abspack scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.634
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3601
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2503
_reflns_number_total             3601
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00659b2.cif
_cod_data_source_block           I4883
_cod_depositor_comments
'Adding full bibliography for 7243129--7243133.cif.'
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_original_formula_sum        'C14.50 H11.50 N1.50 Ni0.75 O6.62'
_cod_database_code               7243131
_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. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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_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
Ni1 Ni 0.250000 0.750000 0.250000 0.0288(3) Uani 1 2 d S . P . .
Ni2 Ni 0.000000 0.500000 0.500000 0.0451(4) Uani 1 4 d S T P . .
O1 O 0.1895(3) 0.70134(11) 0.1137(3) 0.0383(8) Uani 1 1 d . . . . .
O2 O 0.4406(3) 0.75068(10) 0.2709(3) 0.0352(8) Uani 1 1 d . . . . .
O4 O 0.1885(5) 0.500000 0.5152(6) 0.0556(14) Uani 1 2 d S T P . .
O3 O 0.4233(3) 0.69822(13) 0.1363(3) 0.0479(9) Uani 1 1 d . . . . .
N1 N 0.2836(4) 0.69392(12) 0.3555(4) 0.0341(8) Uani 1 1 d . . . . .
O5 O 0.1405(6) 0.500000 0.3201(6) 0.0749(18) Uani 1 2 d S T P . .
O6 O 0.0834(7) 0.500000 0.6868(6) 0.109(3) Uani 1 2 d S T P . .
N2 N 0.000000 0.5681(2) 0.500000 0.0639(18) Uani 1 2 d S T P . .
C1 C 0.3487(5) 0.69224(17) 0.4784(5) 0.0438(11) Uani 1 1 d . . . . .
H1 H 0.387163 0.718002 0.522570 0.057 Uiso 1 1 calc R U . . .
C2 C 0.3593(7) 0.6531(2) 0.5400(6) 0.0655(17) Uani 1 1 d . . . . .
H2 H 0.405956 0.652345 0.625045 0.085 Uiso 1 1 calc R U . . .
C3 C 0.3021(9) 0.6157(2) 0.4768(7) 0.077(2) Uani 1 1 d . . . . .
H3 H 0.307612 0.589159 0.517964 0.100 Uiso 1 1 calc R U . . .
C4 C 0.2347(7) 0.61730(18) 0.3497(6) 0.0646(17) Uani 1 1 d . . . . .
H4 H 0.195864 0.591726 0.304753 0.084 Uiso 1 1 calc R U . . .
C5 C 0.2260(5) 0.65702(17) 0.2910(5) 0.0434(11) Uani 1 1 d . . . . .
C6 C 0.1525(5) 0.66150(17) 0.1574(5) 0.0482(12) Uani 1 1 d . . . . .
H6A H 0.169262 0.635581 0.119532 0.063 Uiso 1 1 calc R U . . .
H6B H 0.058166 0.662427 0.132850 0.063 Uiso 1 1 calc R U . . .
C7 C 0.4847(4) 0.72863(15) 0.2103(4) 0.0317(9) Uani 1 1 d . . . . .
C8 C 0.6217(5) 0.74023(15) 0.2317(4) 0.0314(9) Uani 1 1 d . . . . .
C9 C 0.6721(4) 0.72080(17) 0.1572(4) 0.0368(10) Uani 1 1 d . . . . .
H9 H 0.620403 0.700755 0.095996 0.048 Uiso 1 1 calc R U . . .
C10 C 0.7016(4) 0.76845(17) 0.3250(4) 0.0374(10) Uani 1 1 d . . . . .
H10 H 0.670460 0.780421 0.376581 0.049 Uiso 1 1 calc R U . . .
C11 C 0.0654(9) 0.5900(3) 0.6044(9) 0.095(2) Uani 1 1 d . U . . .
H11 H 0.113910 0.575154 0.678182 0.123 Uiso 1 1 calc R U . . .
C12 C 0.0581(12) 0.6377(4) 0.5987(15) 0.154(5) Uani 1 1 d . U . . .
H12 H 0.098665 0.653180 0.672439 0.200 Uiso 1 1 calc R U . . .
C13 C 0.000000 0.6608(5) 0.500000 0.194(11) Uani 1 2 d S TU P . .
H13 H -0.000001 0.691829 0.499998 0.252 Uiso 1 2 calc R U P . .
C14 C 0.2183(8) 0.500000 0.4288(8) 0.0483(16) Uani 1 2 d S T P . .
C15 C 0.3648(8) 0.500000 0.4671(8) 0.0479(17) Uani 1 2 d S T P . .
C16 C 0.4577(8) 0.500000 0.5864(9) 0.057(2) Uani 1 2 d S T P . .
H16 H 0.430363 0.500000 0.646954 0.075 Uiso 1 2 calc R U P . .
C17 C 0.5897(9) 0.500000 0.6199(9) 0.061(2) Uani 1 2 d S T P . .
H17 H 0.650561 0.500000 0.702627 0.079 Uiso 1 2 calc R U P . .
O1W O 0.500000 0.000000 0.500000 0.39(7) Uani 0.5 4 d S T P . .
O2W O 0.000000 0.089(3) 0.500000 0.77(4) Uiso 1 2 d S . P . .
O3W O 0.423(12) 0.000000 0.481(16) 0.96(11) Uiso 1 2 d S . P . .
O4W O 0.377(6) 0.055(2) 0.541(5) 0.78(4) 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'
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'
Ni Ni 0.3393 1.1124 '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
N1 Ni1 N1 180.00(12) 7_565 . ?
N1 Ni1 O2 92.93(13) 7_565 7_565 ?
N1 Ni1 O2 87.07(13) . 7_565 ?
N1 Ni1 O2 87.07(13) 7_565 . ?
N1 Ni1 O2 92.93(13) . . ?
O2 Ni1 O2 180.0 7_565 . ?
N1 Ni1 O1 80.21(14) 7_565 7_565 ?
N1 Ni1 O1 99.79(14) . 7_565 ?
O2 Ni1 O1 92.57(12) 7_565 7_565 ?
O2 Ni1 O1 87.43(12) . 7_565 ?
N1 Ni1 O1 99.79(14) 7_565 . ?
N1 Ni1 O1 80.21(14) . . ?
O2 Ni1 O1 87.43(12) 7_565 . ?
O2 Ni1 O1 92.57(12) . . ?
O1 Ni1 O1 180.00(13) 7_565 . ?
O6 Ni2 O6 180.0 . 5_566 ?
O6 Ni2 N2 90.000(1) . . ?
O6 Ni2 N2 90.000(1) 5_566 . ?
O6 Ni2 N2 90.000(1) . 5_566 ?
O6 Ni2 N2 90.000(1) 5_566 5_566 ?
N2 Ni2 N2 180.0 . 5_566 ?
O6 Ni2 O4 88.5(3) . . ?
O6 Ni2 O4 91.5(3) 5_566 . ?
N2 Ni2 O4 90.000(3) . . ?
N2 Ni2 O4 90.000(1) 5_566 . ?
O6 Ni2 O4 91.5(3) . 5_566 ?
O6 Ni2 O4 88.5(3) 5_566 5_566 ?
N2 Ni2 O4 90.000(1) . 5_566 ?
N2 Ni2 O4 90.000(3) 5_566 5_566 ?
O4 Ni2 O4 180.0 . 5_566 ?
C6 O1 Ni1 108.9(3) . . ?
C7 O2 Ni1 127.1(3) . . ?
C14 O4 Ni2 126.7(5) . . ?
C5 N1 C1 119.9(4) . . ?
C5 N1 Ni1 113.9(3) . . ?
C1 N1 Ni1 126.0(3) . . ?
C11 N2 C11 120.5(11) . 2_556 ?
C11 N2 Ni2 119.8(5) . . ?
C11 N2 Ni2 119.8(5) 2_556 . ?
N1 C1 C2 121.0(5) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.2(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.5(5) . . ?
N1 C5 C6 117.2(4) . . ?
C4 C5 C6 122.3(5) . . ?
O1 C6 C5 112.2(4) . . ?
O1 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
O1 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O3 C7 O2 125.0(4) . . ?
O3 C7 C8 118.9(4) . . ?
O2 C7 C8 116.1(4) . . ?
C10 C8 C9 119.1(4) . . ?
C10 C8 C7 121.5(4) . . ?
C9 C8 C7 119.4(4) . . ?
C10 C9 C8 120.1(5) 7_665 . ?
C10 C9 H9 120.0 7_665 . ?
C8 C9 H9 120.0 . . ?
C8 C10 C9 120.8(4) . 7_665 ?
C8 C10 H10 119.6 . . ?
C9 C10 H10 119.6 7_665 . ?
N2 C11 C12 117.0(11) . . ?
N2 C11 H11 121.5 . . ?
C12 C11 H11 121.5 . . ?
C13 C12 C11 125.4(14) . . ?
C13 C12 H12 117.3 . . ?
C11 C12 H12 117.3 . . ?
C12 C13 C12 114.6(16) 2_556 . ?
C12 C13 H13 122.7 2_556 . ?
C12 C13 H13 122.7 . . ?
O5 C14 O4 126.0(7) . . ?
O5 C14 C15 118.8(7) . . ?
O4 C14 C15 115.2(7) . . ?
C16 C15 C17 117.0(7) . 5_666 ?
C16 C15 C14 122.3(7) . . ?
C17 C15 C14 120.7(8) 5_666 . ?
C17 C16 C15 121.8(8) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C15 121.2(9) . 5_666 ?
C16 C17 H17 119.4 . . ?
C15 C17 H17 119.4 5_666 . ?
O3W O1W O3W 180.00(3) 5_656 . ?
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
Ni1 N1 2.051(4) 7_565 ?
Ni1 N1 2.051(4) . ?
Ni1 O2 2.059(3) 7_565 ?
Ni1 O2 2.059(3) . ?
Ni1 O1 2.087(3) 7_565 ?
Ni1 O1 2.087(3) . ?
Ni2 O6 2.042(7) . ?
Ni2 O6 2.042(7) 5_566 ?
Ni2 N2 2.046(7) . ?
Ni2 N2 2.046(7) 5_566 ?
Ni2 O4 2.061(5) . ?
Ni2 O4 2.061(5) 5_566 ?
O1 C6 1.451(6) . ?
O2 C7 1.260(5) . ?
O4 C14 1.256(9) . ?
O3 C7 1.250(5) . ?
N1 C5 1.344(6) . ?
N1 C1 1.343(6) . ?
O5 C14 1.216(10) . ?
N2 C11 1.324(9) . ?
N2 C11 1.324(9) 2_556 ?
C1 C2 1.372(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.349(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.466(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.496(6) . ?
C8 C10 1.377(7) . ?
C8 C9 1.411(6) . ?
C9 C10 1.386(6) 7_665 ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.433(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.285(14) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.505(10) . ?
C15 C16 1.356(12) . ?
C15 C17 1.386(11) 5_666 ?
C16 C17 1.359(11) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
O1W O3W 0.80(14) 5_656 ?
O1W O3W 0.80(14) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 1.0(7) . . . . ?
Ni1 N1 C1 C2 176.5(4) . . . . ?
N1 C1 C2 C3 -1.0(10) . . . . ?
C1 C2 C3 C4 1.1(12) . . . . ?
C2 C3 C4 C5 -1.0(11) . . . . ?
C1 N1 C5 C4 -0.9(7) . . . . ?
Ni1 N1 C5 C4 -177.0(4) . . . . ?
C1 N1 C5 C6 177.8(4) . . . . ?
Ni1 N1 C5 C6 1.8(5) . . . . ?
C3 C4 C5 N1 0.9(9) . . . . ?
C3 C4 C5 C6 -177.8(6) . . . . ?
Ni1 O1 C6 C5 -29.2(5) . . . . ?
N1 C5 C6 O1 19.0(6) . . . . ?
C4 C5 C6 O1 -162.3(5) . . . . ?
Ni1 O2 C7 O3 -9.3(7) . . . . ?
Ni1 O2 C7 C8 171.4(3) . . . . ?
O3 C7 C8 C10 -170.0(5) . . . . ?
O2 C7 C8 C10 9.4(7) . . . . ?
O3 C7 C8 C9 8.0(7) . . . . ?
O2 C7 C8 C9 -172.6(4) . . . . ?
C10 C8 C9 C10 -2.6(8) . . . 7_665 ?
C7 C8 C9 C10 179.4(4) . . . 7_665 ?
C9 C8 C10 C9 2.6(8) . . . 7_665 ?
C7 C8 C10 C9 -179.4(4) . . . 7_665 ?
C11 N2 C11 C12 1.9(6) 2_556 . . . ?
Ni2 N2 C11 C12 -178.1(6) . . . . ?
N2 C11 C12 C13 -4.4(14) . . . . ?
C11 C12 C13 C12 2.2(7) . . . 2_556 ?
Ni2 O4 C14 O5 0.000(3) . . . . ?
Ni2 O4 C14 C15 180.000(2) . . . . ?
O5 C14 C15 C16 180.000(3) . . . . ?
O4 C14 C15 C16 0.000(4) . . . . ?
O5 C14 C15 C17 0.000(3) . . . 5_666 ?
O4 C14 C15 C17 180.000(3) . . . 5_666 ?
C17 C15 C16 C17 0.000(4) 5_666 . . . ?
C14 C15 C16 C17 180.000(4) . . . . ?
C15 C16 C17 C15 0.000(4) . . . 5_666 ?
