The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
Li, Na; Wang, Xiao-Jie; Qin, Yu-Cai; Wang, Jing-Yun; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 585–587; doi:10.1515/ncrs-2023-0110

data_8107502
_publ_section_title
;
 The crystal structure of tetra(1-ethylimidazole-\k 1 N)-[\m
 4-imidazole-4,5-dicarboxylato-\k 4 O, N, O&#x2032;,
 N&#x2032;]-trioxido-divanadium, C25H33N10O7V2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              585
_journal_page_last               587
_journal_paper_doi               10.1515/ncrs-2023-0110
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C25 H33 N10 O7 V2'
_chemical_formula_sum            'C25 H33 N10 O7 V2'
_chemical_formula_weight         687.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                65.3730(10)
_cell_angle_beta                 70.3510(10)
_cell_angle_gamma                88.052(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3933(4)
_cell_length_b                   12.5655(5)
_cell_length_c                   14.1841(5)
_cell_measurement_reflns_used    4598
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.93
_cell_volume                     1573.62(11)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015) [3]'
_computing_structure_solution    'Bruker SHELXTL [4]'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13171
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.361
_diffrn_reflns_theta_min         2.926
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6678
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0362
_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/[\s^2^(Fo^2^)+(0.0291P)^2^+0.9293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4326
_reflns_number_total             5733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0110_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        1573.62(10)
_cod_database_code               8107502
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C10 = C19-C20 = C9'-C10' = C19'-C20'
 1.53 with sigma of 0.02
 N4-C9 \\sim N4-C9' \\sim N8-C19 \\sim N8-C19'
 with sigma of 0.02
 N4-C10 \\sim N4-C10' \\sim N8-C20 \\sim N8-C20'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10 \\sim C9' \\sim C10' \\sim C19 \\sim C20 \\sim C19' \\sim C20':
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.03 within 2A
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(C10')=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C24(H24A,H24B), C9(H9A,H9B), C9'(H9'A,H9'B), C19(H19A,H19B),
 C19'(H19C,H19D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C10(H10A,H10B,H10C), C10'(H10D,H10E,
 H10F), C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F)
;
_shelx_res_checksum              53924
_shelx_hkl_checksum              98079
_olex2_submission_special_instructions 'No special instructions were received'