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_1568960
_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         'C22 H36 N2 O25 V6, 2(C16 H36 N), 2(C H Cl3)'
_chemical_formula_sum            'C56 H110 Cl6 N4 O25 V6'
_chemical_formula_weight         1757.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-12
_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                90
_cell_angle_beta                 90.0190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.63100(10)
_cell_length_b                   19.7400(2)
_cell_length_c                   18.5098(2)
_cell_measurement_reflns_used    7001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5270
_cell_measurement_theta_min      3.2380
_cell_volume                     3884.39(7)
_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 0.965
_diffrn_measured_fraction_theta_max 0.929
_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    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-120.00   81
  2  \w     27.00  98.00   1.00    1.00    --   41.68-125.00-150.00   71
  3  \w      6.00  83.00   1.00    1.00    --   41.68 -99.00-120.00   77
  4  \w    103.00 178.00   1.00    4.00    --  106.01  77.00-150.00   75
  5  \w    104.00 178.00   1.00    4.00    --  106.01 108.00 109.00   74
  6  \w     77.00 178.00   1.00    4.00    --  106.01  61.00   0.00  101
  7  \w     33.00 112.00   1.00    4.00    --  106.01-125.00-150.00   79
  8  \w     80.00 178.00   1.00    4.00    --  106.01  45.00 -60.00   98
  9  \w   -114.00 -12.00   1.00    1.00    --  -41.68 -65.00  94.00  102
 10  \w   -115.00 -86.00   1.00    1.00    --  -41.68 -57.00 -30.00   29
 11  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-150.00  101
;
_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      0.0695678000
_diffrn_orient_matrix_UB_12      0.0394353000
_diffrn_orient_matrix_UB_13      -0.0596577000
_diffrn_orient_matrix_UB_21      0.1224132000
_diffrn_orient_matrix_UB_22      -0.0379981000
_diffrn_orient_matrix_UB_23      0.0186265000
_diffrn_orient_matrix_UB_31      -0.0343650000
_diffrn_orient_matrix_UB_32      -0.0555903000
_diffrn_orient_matrix_UB_33      -0.0549610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19898
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.831
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.333
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.687
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0267P)^2^+1.4836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6027
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00038a2.cif
_cod_data_source_block           am49
_cod_depositor_comments
'Adding full bibliography for 1568959--1568960.cif.'
_cod_database_code               1568960
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H110 Cl6 N4 O25 V6'
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.148
_reflns_odcompleteness_completeness 96.33
_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 Ternary CH refined with riding coordinates:
 C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              65859
_shelx_hkl_checksum              14867
_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 2.374
_oxdiff_exptl_absorpt_empirical_full_min 0.670