Synthesis and characterization of an organic-inorganic hybrid crystal: 2[Co(en)<sub>3</sub>](V<sub>4</sub>O<sub>13</sub>)·4H<sub>2</sub>O.
Vosegaard, Emilie Skytte; Mamakhel, Mohammad Aref Hasen; Parmar, Vijay Singh; Bertelsen, Andreas Dueholm; Iversen, Bo Brummerstedt; Acta crystallographica Section B, Structural science, crystal engineering and materials 80 (2024) 488–494; doi:10.1107/S2052520624007509

data_2312623
_publ_section_title
;
 Synthesis and characterization of an organic-inorganic hybrid crystal:
 2[Co(en)<sub>3</sub>](V<sub>4</sub>O<sub>13</sub>)&#xb7;4H<sub>2</sub>O.
;
_journal_coeditor_code           LO5123SUP1
_journal_issue                   5
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              488
_journal_page_last               494
_journal_paper_doi               10.1107/S2052520624007509
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         '2(C6 H24 Co N6), O13 V4, 4(H2 O)'
_chemical_formula_sum            'C12 H56 Co2 N12 O17 V4'
_chemical_formula_weight         962.30
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-04 deposited with the CCDC. 2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                81.491(3)
_cell_angle_beta                 71.357(3)
_cell_angle_gamma                65.064(4)
_cell_formula_units_Z            1
_cell_length_a                   8.6226(3)
_cell_length_b                   8.9645(3)
_cell_length_c                   12.8206(5)
_cell_measurement_reflns_used    21505
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0240
_cell_measurement_theta_min      2.4880
_cell_volume                     851.36(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -19.00  37.00   0.50   30.00    --   -6.20  19.00  83.00  112
  2  \w    -56.00 -30.00   0.50   30.00    --   -6.20 -19.00 -83.00   52
  3  \w    -67.00  26.00   0.50   30.00    --    6.67 -19.00 -83.00  186
  4  \w     -5.00  65.00   0.50   30.00    --    6.67  19.00  83.00  140
  5  \w    -64.00 -24.00   0.50   30.00    --   -6.20 123.00   5.75   80
  6  \w    -66.00 -18.00   0.50   30.00    --   -6.20 127.00-144.71   96
  7  \w    -60.00  -6.00   0.50   30.00    --   -6.20 115.00 155.33  108
  8  \w     23.00  76.00   0.50   30.00    --    6.67  77.00 -90.00  106
  9  \w    -12.00  76.00   0.50   30.00    --    6.67  38.00 120.00  176
 10  \w    -73.00  26.00   0.50   30.00    --    6.67 -19.00  90.00  198
 11  \w     -1.00  48.00   0.50   30.00    --    6.67 -99.00   0.00   98
 12  \w    -22.00  69.00   0.50   30.00    --    6.67  77.00-150.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0779191000
_diffrn_orient_matrix_UB_12      -0.0132817000
_diffrn_orient_matrix_UB_13      0.0142050000
_diffrn_orient_matrix_UB_21      0.0249217000
_diffrn_orient_matrix_UB_22      -0.0862156000
_diffrn_orient_matrix_UB_23      0.0003357000
_diffrn_orient_matrix_UB_31      0.0477002000
_diffrn_orient_matrix_UB_32      -0.0024616000
_diffrn_orient_matrix_UB_33      -0.0566408000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.011
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       plate
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.1775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4778
_reflns_number_total             5099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5123.cif
_cod_data_source_block           I
_cod_depositor_comments
;
         Adding full bibliography for 2312623.cif.

2025-06-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         481.15
_cod_original_formula_moiety         'C6 H24 Co N6, O6.5 V2, 2(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C6 H28 Co N6 O8.50 V2'
_cod_database_code               2312623
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Co(C2H2N2H2)3(V2O6.5)
_chemical_oxdiff_usercomment     150K
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N4(H4A,H4B), N3(H3A,H3B), N6(H6A,H6B), N1(H1A,H1B), N2(H2A,H2B),
 C3(H3C,H3D), C4(H4C,H4D), C1(H1C,H1D), C5(H5C,H5D), C6(H6C,H6D), C2(H2C,H2D)
;
_shelx_res_checksum              16586
_shelx_hkl_checksum              77648
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.817