Rational synthesis of elusive organic-inorganic hybrid metal-oxo clusters: formation and post-functionalization of hexavanadates.
Salazar Marcano, David E.; Kalandia, Givi; Moussawi, Mhamad Aly; Van Hecke, Kristof; Parac-Vogt, Tatjana N; Chemical science 14 (2023) 5405–5414; doi:10.1039/d3sc00038a

data_1568959
_publ_section_title
;
 Rational synthesis of elusive organic-inorganic hybrid metal-oxo
 clusters: formation and post-functionalization of hexavanadates.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5405
_journal_page_last               5414
_journal_paper_doi               10.1039/d3sc00038a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C12 H18 Cl2 N2 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C44 H90 Cl2 N4 O21 V6'
_chemical_formula_weight         1387.74
_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             2021-03-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                112.102(6)
_cell_angle_beta                 97.669(5)
_cell_angle_gamma                93.798(5)
_cell_formula_units_Z            1
_cell_length_a                   10.7293(6)
_cell_length_b                   11.8938(8)
_cell_length_c                   12.7361(8)
_cell_measurement_reflns_used    3899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7340
_cell_measurement_theta_min      3.7750
_cell_volume                     1480.33(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00  90.00   99
  2  \w    -66.00  33.00   1.00    2.00    --  -41.68  38.00 -90.00   99
  3  \w      7.00  34.00   1.00    2.00    --   41.68  83.00  96.38   27
  4  \w     27.00  98.00   1.00    2.00    --   41.68-125.00 -60.00   71
  5  \w    -30.00  70.00   1.00    2.00    --   41.68 -57.00 -30.00  100
  6  \w    103.00 178.00   1.00    6.00    --  106.01  77.00  30.00   75
  7  \w     33.00 132.00   1.00    6.00    --  106.01 -45.00 120.00   99
  8  \w    103.00 178.00   1.00    6.00    --  106.01  77.00-180.00   75
  9  \w     30.00 139.00   1.00    6.00    --  106.01 -77.00   0.00  109
 10  \w     33.00 112.00   1.00    6.00    --  106.01-125.00 -30.00   79
 11  \w     78.00 178.00   1.00    6.00    --  106.01  30.00 -30.00  100
 12  \w     33.00 132.00   1.00    6.00    --  106.01 -45.00-120.00   99
 13  \w     23.00 107.00   1.00    6.00    --  106.01 -94.00   0.00   84
 14  \w     78.00 178.00   1.00    6.00    --  106.01  30.00 120.00  100
 15  \w     33.00 112.00   1.00    6.00    --  106.01-125.00 120.00   79
 16  \w     23.00 107.00   1.00    6.00    --  106.01 -94.00 150.00   84
 17  \w     23.00 107.00   1.00    6.00    --  106.01 -94.00-150.00   84
 18  \w   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00 -90.00  101
 19  \w   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00 -30.00   99
 20  \w      8.00  42.00   1.00    2.00    --   41.68  82.00-130.74   34
 21  \w      9.00  42.00   1.00    2.00    --   41.68  80.00  31.74   33
 22  \w      7.00  34.00   1.00    2.00    --   41.68  83.00 -96.37   27
 23  \w     78.00 178.00   1.00    6.00    --  106.01  57.00  26.76  100
 24  \w     76.00 178.00   1.00    6.00    --  106.01  64.00-141.38  102
 25  \w     53.00 178.00   1.00    6.00    --  106.01  15.00-120.00  125
 26  \w     77.00 178.00   1.00    6.00    --  106.01  59.00  50.24  101
 27  \w     80.00 178.00   1.00    6.00    --  106.01  45.00   0.00   98
 28  \w     76.00 178.00   1.00    6.00    --  106.01  65.00 131.38  102
 29  \w     77.00 178.00   1.00    6.00    --  106.01  61.00-180.00  101
 30  \w     78.00 178.00   1.00    6.00    --  106.01  57.00 -41.30  100
 31  \w     77.00 178.00   1.00    6.00    --  106.01  61.00 120.00  101
 32  \w     77.00 178.00   1.00    6.00    --  106.01  60.00-101.64  101
 33  \w      6.00  83.00   1.00    2.00    --   41.68 -99.00 120.00   77
 34  \w      7.00  33.00   1.00    2.00    --   41.68  84.00 138.78   26
 35  \w      8.00  42.00   1.00    2.00    --   41.68  81.00-178.95   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394903000
_diffrn_orient_matrix_UB_12      0.0873512000
_diffrn_orient_matrix_UB_13      -0.0585997000
_diffrn_orient_matrix_UB_21      -0.0146155000
_diffrn_orient_matrix_UB_22      0.0968309000
_diffrn_orient_matrix_UB_23      0.1172549000
_diffrn_orient_matrix_UB_31      0.1398579000
_diffrn_orient_matrix_UB_32      0.0534475000
_diffrn_orient_matrix_UB_33      0.0194125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27888
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.068
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0784P)^2^+0.2053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4169
_reflns_number_total             5919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00038a2.cif
_cod_data_source_block           exp_1670
_cod_depositor_comments
'Adding full bibliography for 1568959--1568960.cif.'
_cod_database_code               1568959
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N2 O2 Cl1 V10'
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.435
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 N1-H1
 0.88 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              3150
_shelx_hkl_checksum              94893
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.673