The crystal structure of tetrakis(1-isopropylimidazole-κ1 N)-[μ2- imidazole-4,5-dicarboxylato-κ4 O,N,O′,N′)]- trioxido-divanadium, C29H41N10O7V2
Ren, Xiang-Yu; Wang, Xiao-Jie; Qin, Yu-Cai; Tong, Yue; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 803–805; doi:10.1515/ncrs-2023-0223

data_8107568
_publ_section_title
;
 The crystal structure of tetrakis(1-isopropylimidazole-\k1 N)-[\m2-
 imidazole-4,5-dicarboxylato-\k4 O,N,O&#x2032;,N&#x2032;)]-
 trioxido-divanadium, C29H41N10O7V2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              803
_journal_page_last               805
_journal_paper_doi               10.1515/ncrs-2023-0223
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C29 H41 N10 O7 V2'
_chemical_formula_sum            'C29 H41 N10 O7 V2'
_chemical_formula_weight         743.60
_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
_atom_sites_solution_primary     dual
_cell_angle_alpha                111.6090(10)
_cell_angle_beta                 108.7020(10)
_cell_angle_gamma                93.957(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3461(5)
_cell_length_b                   12.7013(5)
_cell_length_c                   14.0649(5)
_cell_measurement_reflns_used    4174
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1744.19(12)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016) [1]'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'XL (Sheldrick, 2015b) [3]'
_computing_structure_solution    'XT (Sheldrick, 2015a) [4]'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14702
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.373
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0392P)^2^+2.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4640
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0223_Suppl_001.cif
_cod_data_source_block           33
_cod_original_cell_volume        1744.20(12)
_cod_database_code               8107568
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C11-C23'
 1.5 with sigma of 0.01
 C9-C3
 1.5 with sigma of 0.01
 C9-C7
 1.5 with sigma of 0.01
3. Rigid bond restraints
 N9, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C11 \\sim C23' \\sim C23: within 3.2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 3.2A
C3 \\sim C9: within 3.8A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 3.8A
C9 \\sim C7: within 3.8A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 3.8A
C9 \\sim C3: within 3.8A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 3.8A
C19 \\sim C27 \\sim C13: within 3.2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 3.2A
Uanis(C7) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: H29A(0.75) H29B(0.75) H29C(0.75) H29D(0.25) H29E(0.25) H29F(0.25)
 H11A(0.75) H11B(0.75) H11C(0.75) H11D(0.25) H11E(0.25) H11F(0.25) C23'(0.75)
 H23'(0.75) C23(0.25) H23(0.25)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C9(H9), C19(H19), C23'(H23'), C23(H23)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C14(H14), C16(H16), C18(H18), C20(H20), C22(H22), C24(H24),
 C26(H26), C28(H28), C2(H2), C17(H17), C21(H21)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C29(H29D,H29E,H29F), C5(H5A,H5B,H5C), C11(H11A,H11B,
 H11C), C11(H11D,H11E,H11F), C3(H3A,H3B,H3C), C25(H25A,H25B,H25C), C13(H13A,
 H13B,H13C), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              22401
_shelx_hkl_checksum              27780
_olex2_submission_special_instructions 'No special instructions were received'