#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:15:17 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303736 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/95/7719546.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_7719546
loop_
_publ_author_name
'Simran, Simran'
'Tansky, Maxym'
'Trabulsi, Seth'
'Deng, Liangzi'
'Chu, Ching-Wu'
'Ozarowski, Andrew'
'Comito, Robert J.'
_publ_section_title
;
 Cooperative enhancement of redox catalysis in divanadium complexes
 binucleated by 1,8-naphthyridine-2,7-dicarboxylate.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15400
_journal_page_last               15405
_journal_paper_doi               10.1039/d5dt01296a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C22.696 N4 O8 V2'
_chemical_formula_sum            'C22.7 H21.39 N4 O8 V2'
_chemical_formula_weight         580.07
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2n3gnx
_audit_creation_date             2024-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-23 deposited with the CCDC.	2025-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.413(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8965(12)
_cell_length_b                   9.8187(6)
_cell_length_c                   12.6691(8)
_cell_measurement_reflns_used    2895
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.41
_cell_measurement_theta_min      4.45
_cell_volume                     2472.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'narrow frame omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8013
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.471
_diffrn_reflns_theta_max         67.471
_diffrn_reflns_theta_min         4.448
_exptl_absorpt_coefficient_mu    6.823
_exptl_absorpt_correction_T_max  0.8171
_exptl_absorpt_correction_T_min  0.6044
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       needle
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2149
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0407
_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)+(0.0846P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1864
_reflns_number_total             2149
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01296a2.cif
_cod_data_source_block           cu_XW643_0m_a
_cod_depositor_comments
'Adding full bibliography for 7719545--7719549.cif.'
_cod_original_formula_sum        'C22.70 H21.39 N4 O8 V2'
_cod_database_code               7719546
_shelx_shelxl_version_number     2019/3
_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_max   0.876
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Restrained distances
 O4-C12 \\sim O4-C12'
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C12')
3. Others
 Sof(C12')=Sof(H12D)=Sof(H12E)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
V1 V 0.56089(2) 0.17619(4) 0.68077(3) 0.02078(18) Uani 1 1 d . . . . .
O1 O 0.58149(8) 0.25114(16) 0.53593(13) 0.0271(4) Uani 1 1 d . . . . .
O2 O 0.61622(9) 0.42838(18) 0.44126(15) 0.0359(4) Uani 1 1 d . . . . .
O3 O 0.58018(8) 0.02115(16) 0.65785(14) 0.0270(4) Uani 1 1 d . . . . .
O4 O 0.53984(8) 0.16817(15) 0.83253(13) 0.0227(4) Uani 1 1 d D . . . .
N1 N 0.53288(9) 0.40748(18) 0.67782(15) 0.0216(4) Uani 1 1 d . . . . .
N2 N 0.65871(9) 0.25093(19) 0.72538(16) 0.0258(5) Uani 1 1 d . . . . .
C1 C 0.56098(11) 0.4724(2) 0.6005(2) 0.0256(5) Uani 1 1 d . . . . .
C2 C 0.56261(12) 0.6155(2) 0.5924(2) 0.0293(5) Uani 1 1 d . . . . .
C3 C 0.53326(12) 0.6915(2) 0.6679(2) 0.0286(6) Uani 1 1 d . . . . .
C4 C 0.500000 0.6255(3) 0.750000 0.0240(7) Uani 1 2 d S T P . .
C5 C 0.500000 0.4811(3) 0.750000 0.0225(7) Uani 1 2 d S T P . .
C6 C 0.58971(12) 0.3788(2) 0.51784(19) 0.0267(5) Uani 1 1 d . . . . .
C7 C 0.66952(13) 0.3311(2) 0.8106(2) 0.0322(6) Uani 1 1 d . . . . .
C8 C 0.73253(14) 0.3736(3) 0.8447(3) 0.0434(7) Uani 1 1 d . . . . .
C9 C 0.78750(14) 0.3321(3) 0.7892(3) 0.0499(9) Uani 1 1 d . . . . .
C10 C 0.77716(14) 0.2517(3) 0.7009(3) 0.0472(8) Uani 1 1 d . . . . .
C11 C 0.71226(13) 0.2142(3) 0.6712(2) 0.0356(6) Uani 1 1 d . . . . .
C12 C 0.5713(18) 0.076(2) 0.908(2) 0.034(3) Uani 0.652(10) 1 d D . P A 1
C12' C 0.569(3) 0.063(5) 0.899(4) 0.034(3) Uani 0.348(10) 1 d D . P A 2
C13 C 0.6396(4) 0.0594(9) 0.9237(8) 0.043(3) Uani 0.348(10) 1 d . . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2025-ksrvb 2025
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
O1 V1 V1 135.53(5) . 2_656 ?
O1 V1 N1 72.02(6) . . ?
O1 V1 N2 84.17(7) . . ?
O3 V1 V1 107.87(6) . 2_656 ?
O3 V1 O1 96.98(8) . . ?
O3 V1 O4 101.53(8) . . ?
O3 V1 O4 101.18(7) . 2_656 ?
O3 V1 N1 168.61(8) . . ?
O3 V1 N2 98.76(8) . . ?
O4 V1 V1 40.40(4) . 2_656 ?
O4 V1 V1 39.94(5) 2_656 2_656 ?
O4 V1 O1 100.19(7) 2_656 . ?
O4 V1 O1 161.07(6) . . ?
O4 V1 O4 80.16(7) . 2_656 ?
O4 V1 N1 78.47(6) 2_656 . ?
O4 V1 N1 89.66(6) . . ?
O4 V1 N2 158.87(7) 2_656 . ?
O4 V1 N2 89.11(7) . . ?
N1 V1 V1 79.32(5) . 2_656 ?
N2 V1 V1 125.83(6) . 2_656 ?
N2 V1 N1 83.36(7) . . ?
C6 O1 V1 123.04(15) . . ?
V1 O4 V1 99.66(7) . 2_656 ?
C12 O4 V1 124.5(15) . . ?
C12 O4 V1 119.1(16) . 2_656 ?
C12' O4 V1 120(3) . . ?
C1 N1 V1 112.01(15) . . ?
C1 N1 C5 118.5(2) . . ?
C5 N1 V1 128.97(16) . . ?
C7 N2 V1 121.78(17) . . ?
C11 N2 V1 120.48(17) . . ?
C11 N2 C7 117.7(2) . . ?
N1 C1 C2 123.4(2) . . ?
N1 C1 C6 113.8(2) . . ?
C2 C1 C6 122.8(2) . . ?
C3 C2 C1 118.9(2) . . ?
C2 C3 C4 119.5(2) . . ?
C3 C4 C3 125.5(3) . 2_656 ?
C3 C4 C5 117.27(15) . . ?
C3 C4 C5 117.27(15) 2_656 . ?
N1 C5 N1 115.5(3) . 2_656 ?
N1 C5 C4 122.25(14) 2_656 . ?
N1 C5 C4 122.25(14) . . ?
O1 C6 C1 114.3(2) . . ?
O2 C6 O1 126.2(2) . . ?
O2 C6 C1 119.4(2) . . ?
N2 C7 C8 122.8(3) . . ?
C7 C8 C9 118.7(3) . . ?
C10 C9 C8 119.1(3) . . ?
C9 C10 C11 118.7(3) . . ?
N2 C11 C10 122.9(3) . . ?
C13 C12' O4 121(4) . . ?
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
V1 V1 3.0508(8) 2_656 ?
V1 O1 2.0347(17) . ?
V1 O3 1.5995(16) . ?
V1 O4 1.9866(17) . ?
V1 O4 2.0058(15) 2_656 ?
V1 N1 2.3383(18) . ?
V1 N2 2.1338(19) . ?
O1 C6 1.286(3) . ?
O2 C6 1.225(3) . ?
O4 C12 1.441(8) . ?
O4 C12' 1.435(14) . ?
N1 C1 1.314(3) . ?
N1 C5 1.356(3) . ?
N2 C7 1.346(3) . ?
N2 C11 1.341(3) . ?
C1 C2 1.409(3) . ?
C1 C6 1.523(3) . ?
C2 C3 1.363(4) . ?
C3 C4 1.413(3) . ?
C4 C5 1.418(5) . ?
C7 C8 1.373(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.377(5) . ?
C10 C11 1.380(4) . ?
C12' C13 1.43(6) . ?
