#------------------------------------------------------------------------------
#$Date: 2025-02-01 09:07:15 +0200 (Sat, 01 Feb 2025) $
#$Revision: 297561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/68/7246820.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_7246820
loop_
_publ_author_name
'Bawa, Rashim'
'Negi, Swati'
'Singh, Bholey'
'Pani, Balaram'
'Kumar, Rakesh'
_publ_section_title
;
 A pyridine dicarboxylate based hydrazone Schiff base for reversible
 colorimetric recognition of Ni2+ and PPi
;
_journal_issue                   23
_journal_name_full               'RSC Advances'
_journal_page_first              15391
_journal_page_last               15400
_journal_paper_doi               10.1039/D3RA02021E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C26 H24 N4 O8'
_chemical_formula_weight         520.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-11 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.855(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2016(5)
_cell_length_b                   18.2857(12)
_cell_length_c                   18.8379(13)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.23
_cell_volume                     2457.4(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.1322
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10693
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         6.139
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       rod
_exptl_crystal_F_000             1078
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.007(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.1000
_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)+(0.1000P)²+0.1729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2492
_refine_ls_wR_factor_ref         0.2784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3494
_reflns_number_total             5644
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ra02021e2.cif
_cod_data_source_block           VS132_0m_a
_cod_depositor_comments
;

2025-01-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C H N O'
_cod_original_formula_weight         43.03
_cod_original_formula_units_Z            49
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7246820
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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
O4 O 0.1727(3) 0.26169(15) 0.20375(14) 0.0230(6) Uani 1 1 d . . . . .
O6 O 0.6337(4) 0.50659(14) 0.29730(15) 0.0250(6) Uani 1 1 d . . . . .
O5 O 0.3893(4) 0.53546(14) 0.35476(15) 0.0237(6) Uani 1 1 d . . . . .
N2 N 0.6995(4) 0.48027(16) 0.46407(17) 0.0191(6) Uani 1 1 d . . . . .
N3 N 0.4966(4) 0.30748(17) 0.42662(17) 0.0196(7) Uani 1 1 d . . . . .
N1 N 0.7864(4) 0.51884(17) 0.52071(17) 0.0205(7) Uani 1 1 d . . . . .
H1 H 0.791395 0.502407 0.564834 0.025 Uiso 1 1 calc R U . . .
O1 O 0.9821(4) 0.73081(17) 0.48944(18) 0.0409(8) Uani 1 1 d . . . . .
H1A H 0.871288 0.745571 0.479095 0.061 Uiso 1 1 calc R U . . .
O2 O 0.8622(4) 0.60578(17) 0.44403(17) 0.0366(8) Uani 1 1 d . . . . .
O7 O 0.1769(5) 0.54331(19) -0.00109(18) 0.0442(9) Uani 1 1 d . . . . .
O3 O 0.4363(4) 0.19463(18) 0.22060(19) 0.0425(9) Uani 1 1 d . . . . .
O8 O 0.3224(6) 0.4523(2) -0.04213(19) 0.0514(10) Uani 1 1 d . . . . .
C9 C 0.5294(4) 0.37753(19) 0.41488(19) 0.0168(7) Uani 1 1 d . . . . .
C10 C 0.4837(4) 0.4107(2) 0.3471(2) 0.0190(7) Uani 1 1 d . . . . .
C8 C 0.6234(4) 0.4192(2) 0.4772(2) 0.0184(7) Uani 1 1 d . . . . .
H8 H 0.626999 0.401458 0.524739 0.022 Uiso 1 1 calc R U . . .
C14 C 0.4187(5) 0.3663(2) 0.2890(2) 0.0187(7) Uani 1 1 d . . . . .
N4 N 0.2633(5) 0.4854(2) 0.0073(2) 0.0360(9) Uani 1 1 d . . . . .
C11 C 0.4986(5) 0.4912(2) 0.33607(19) 0.0199(7) Uani 1 1 d . . . . .
C15 C 0.3955(5) 0.2917(2) 0.3015(2) 0.0194(7) Uani 1 1 d . . . . .
C7 C 0.8658(5) 0.5841(2) 0.5065(2) 0.0236(8) Uani 1 1 d . . . . .
C16 C 0.4298(5) 0.2649(2) 0.3719(2) 0.0213(8) Uani 1 1 d . . . . .
C22 C 0.2442(5) 0.4521(2) 0.2003(2) 0.0215(8) Uani 1 1 d . . . . .
H22 H 0.178076 0.469382 0.237252 0.026 Uiso 1 1 calc R U . . .
C6 C 0.9543(5) 0.6279(2) 0.5682(2) 0.0225(8) Uani 1 1 d . . . . .
C21 C 0.3778(5) 0.3975(2) 0.2152(2) 0.0209(8) Uani 1 1 d . . . . .
C1 C 1.0045(5) 0.7007(2) 0.5560(2) 0.0263(9) Uani 1 1 d . . . . .
C23 C 0.4741(5) 0.3720(2) 0.1606(2) 0.0239(8) Uani 1 1 d . . . . .
H23 H 0.567141 0.335263 0.170807 0.029 Uiso 1 1 calc R U . . .
C5 C 0.9956(5) 0.5990(2) 0.6375(2) 0.0239(8) Uani 1 1 d . . . . .
H5 H 0.968647 0.549122 0.645984 0.029 Uiso 1 1 calc R U . . .
C3 C 1.1165(5) 0.7145(2) 0.6813(2) 0.0277(9) Uani 1 1 d . . . . .
H3 H 1.169560 0.744249 0.720168 0.033 Uiso 1 1 calc R U . . .
C24 C 0.2057(5) 0.4819(2) 0.1319(2) 0.0258(8) Uani 1 1 d . . . . .
H24 H 0.114712 0.519337 0.121377 0.031 Uiso 1 1 calc R U . . .
C18 C 0.3386(5) 0.2425(2) 0.2389(2) 0.0249(8) Uani 1 1 d . . . . .
C26 C 0.3046(6) 0.4548(2) 0.0801(2) 0.0264(9) Uani 1 1 d . . . . .
C4 C 1.0752(5) 0.6424(2) 0.6935(2) 0.0298(9) Uani 1 1 d . . . . .
H4 H 1.101471 0.622567 0.740429 0.036 Uiso 1 1 calc R U . . .
C2 C 1.0822(5) 0.7439(2) 0.6138(2) 0.0315(10) Uani 1 1 d . . . . .
H2 H 1.111164 0.793779 0.606242 0.038 Uiso 1 1 calc R U . . .
C25 C 0.4358(6) 0.3995(2) 0.0925(2) 0.0285(9) Uani 1 1 d . . . . .
H25 H 0.497668 0.381055 0.054782 0.034 Uiso 1 1 calc R U . . .
C19 C 0.1198(5) 0.2281(2) 0.1339(2) 0.0261(8) Uani 1 1 d . . . . .
H19A H 0.102213 0.174755 0.139013 0.031 Uiso 1 1 calc R U . . .
H19B H 0.218311 0.236345 0.102895 0.031 Uiso 1 1 calc R U . . .
C17 C 0.3944(6) 0.1863(2) 0.3907(2) 0.0274(9) Uani 1 1 d . . . . .
H17A H 0.513898 0.162439 0.408017 0.041 Uiso 1 1 calc R U . . .
H17B H 0.333609 0.160688 0.348076 0.041 Uiso 1 1 calc R U . . .
H17C H 0.312813 0.184816 0.428269 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6506(6) 0.5819(2) 0.2737(2) 0.0287(9) Uani 1 1 d . . . . .
H12A H 0.710922 0.612746 0.313528 0.034 Uiso 1 1 calc R U . . .
H12B H 0.525765 0.602583 0.256014 0.034 Uiso 1 1 calc R U . . .
C20 C -0.0600(6) 0.2633(3) 0.1020(3) 0.0416(11) Uani 1 1 d . . . . .
H20A H -0.160801 0.248385 0.128971 0.062 Uiso 1 1 calc R U . . .
H20B H -0.090834 0.248096 0.051912 0.062 Uiso 1 1 calc R U . . .
H20C H -0.046138 0.316643 0.104279 0.062 Uiso 1 1 calc R U . . .
C13 C 0.7695(7) 0.5782(3) 0.2146(3) 0.0413(12) Uani 1 1 d . . . . .
H13A H 0.893493 0.558935 0.233460 0.062 Uiso 1 1 calc R U . . .
H13B H 0.782982 0.627319 0.195141 0.062 Uiso 1 1 calc R U . . .
H13C H 0.710046 0.545952 0.176634 0.062 Uiso 1 1 calc R 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'
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'
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
C18 O4 C19 116.4(3) . . ?
C11 O6 C12 117.9(3) . . ?
C8 N2 N1 117.7(3) . . ?
C9 N3 C16 119.3(3) . . ?
N2 N1 C7 117.4(3) . . ?
N2 N1 H1 121.3 . . ?
C7 N1 H1 121.3 . . ?
C1 O1 H1A 109.5 . . ?
N3 C9 C10 122.8(3) . . ?
N3 C9 C8 115.9(3) . . ?
C10 C9 C8 121.3(3) . . ?
C14 C10 C9 118.2(3) . . ?
C14 C10 C11 119.3(3) . . ?
C9 C10 C11 122.5(3) . . ?
N2 C8 C9 117.1(3) . . ?
N2 C8 H8 121.4 . . ?
C9 C8 H8 121.4 . . ?
C10 C14 C15 118.2(3) . . ?
C10 C14 C21 120.7(3) . . ?
C15 C14 C21 121.1(3) . . ?
O7 N4 O8 123.2(4) . . ?
O7 N4 C26 118.8(4) . . ?
O8 N4 C26 118.0(4) . . ?
O5 C11 O6 124.9(3) . . ?
O5 C11 C10 123.7(3) . . ?
O6 C11 C10 111.0(3) . . ?
C14 C15 C16 119.3(3) . . ?
C14 C15 C18 118.7(3) . . ?
C16 C15 C18 122.0(3) . . ?
O2 C7 N1 120.7(4) . . ?
O2 C7 C6 121.5(3) . . ?
N1 C7 C6 117.8(3) . . ?
N3 C16 C15 121.9(3) . . ?
N3 C16 C17 115.5(3) . . ?
C15 C16 C17 122.7(3) . . ?
C21 C22 C24 120.9(3) . . ?
C21 C22 H22 119.5 . . ?
C24 C22 H22 119.5 . . ?
C5 C6 C1 118.8(4) . . ?
C5 C6 C7 122.7(4) . . ?
C1 C6 C7 118.5(4) . . ?
C22 C21 C23 119.4(4) . . ?
C22 C21 C14 120.4(3) . . ?
C23 C21 C14 120.2(3) . . ?
O1 C1 C2 118.2(4) . . ?
O1 C1 C6 122.2(4) . . ?
C2 C1 C6 119.5(4) . . ?
C25 C23 C21 120.7(4) . . ?
C25 C23 H23 119.6 . . ?
C21 C23 H23 119.6 . . ?
C4 C5 C6 120.5(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C26 C24 C22 117.3(4) . . ?
C26 C24 H24 121.3 . . ?
C22 C24 H24 121.3 . . ?
O3 C18 O4 124.7(4) . . ?
O3 C18 C15 123.8(4) . . ?
O4 C18 C15 111.4(3) . . ?
C24 C26 C25 123.5(4) . . ?
C24 C26 N4 117.8(4) . . ?
C25 C26 N4 118.7(4) . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C23 C25 C26 118.1(4) . . ?
C23 C25 H25 120.9 . . ?
C26 C25 H25 120.9 . . ?
O4 C19 C20 106.6(3) . . ?
O4 C19 H19A 110.4 . . ?
C20 C19 H19A 110.4 . . ?
O4 C19 H19B 110.4 . . ?
C20 C19 H19B 110.4 . . ?
H19A C19 H19B 108.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C12 C13 105.3(3) . . ?
O6 C12 H12A 110.7 . . ?
C13 C12 H12A 110.7 . . ?
O6 C12 H12B 110.7 . . ?
C13 C12 H12B 110.7 . . ?
H12A C12 H12B 108.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
O4 C18 1.332(5) . ?
O4 C19 1.455(5) . ?
O6 C11 1.324(4) . ?
O6 C12 1.458(5) . ?
O5 C11 1.214(4) . ?
N2 C8 1.283(5) . ?
N2 N1 1.358(4) . ?
N3 C9 1.326(4) . ?
N3 C16 1.328(5) . ?
N1 C7 1.366(5) . ?
N1 H1 0.8800 . ?
O1 C1 1.359(5) . ?
O1 H1A 0.8400 . ?
O2 C7 1.239(5) . ?
O7 N4 1.227(5) . ?
O3 C18 1.203(5) . ?
O8 N4 1.234(5) . ?
C9 C10 1.411(5) . ?
C9 C8 1.483(5) . ?
C10 C14 1.391(5) . ?
C10 C11 1.493(5) . ?
C8 H8 0.9500 . ?
C14 C15 1.398(5) . ?
C14 C21 1.495(5) . ?
N4 C26 1.474(6) . ?
C15 C16 1.403(6) . ?
C15 C18 1.495(5) . ?
C7 C6 1.481(6) . ?
C16 C17 1.511(5) . ?
C22 C21 1.389(5) . ?
C22 C24 1.390(6) . ?
C22 H22 0.9500 . ?
C6 C5 1.403(6) . ?
C6 C1 1.405(5) . ?
C21 C23 1.397(5) . ?
C1 C2 1.399(6) . ?
C23 C25 1.371(6) . ?
C23 H23 0.9500 . ?
C5 C4 1.381(6) . ?
C5 H5 0.9500 . ?
C3 C2 1.372(7) . ?
C3 C4 1.378(6) . ?
C3 H3 0.9500 . ?
C24 C26 1.376(6) . ?
C24 H24 0.9500 . ?
C26 C25 1.382(6) . ?
C4 H4 0.9500 . ?
C2 H2 0.9500 . ?
C25 H25 0.9500 . ?
C19 C20 1.497(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C12 C13 1.495(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
