Tunable bandgaps in self-assembled transition metal-incorporated heterometallic M<sub>2</sub>Sb<sub>4</sub> (M = V, Mn, Co, Ni, and Cu) oxo clusters.
Navaneetha, Tokala; Ugandhar, Uppara; Samuel, Calvin; Guizouarn, Thierry; Pointillart, Fabrice; Raghunathan, Rajamani; Baskar, Viswanathan; Dalton transactions (Cambridge, England : 2003) 52 (2023) 9328–9336; doi:10.1039/d3dt01000g

data_7713434
_publ_section_title
;
 Tunable bandgaps in self-assembled transition metal-incorporated
 heterometallic M<sub>2</sub>Sb<sub>4</sub> (M = V, Mn, Co, Ni, and Cu)
 oxo clusters.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9328
_journal_page_last               9336
_journal_paper_doi               10.1039/d3dt01000g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C44 H64 Cl4 O22 P4 Sb4 V2'
_chemical_formula_sum            'C44 H64 Cl4 O22 P4 Sb4 V2'
_chemical_formula_weight         1799.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-15
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.005(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9319(2)
_cell_length_b                   24.0942(5)
_cell_length_c                   13.5380(2)
_cell_measurement_reflns_used    17657
_cell_measurement_temperature    109(3)
_cell_measurement_theta_max      26.8040
_cell_measurement_theta_min      2.2400
_cell_volume                     3199.73(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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      109(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -37.00  12.00   0.50   20.00    --  -14.97 -61.00  60.00   98
  2  \w    -41.00  47.00   0.50   20.00    --   16.22 -77.00  60.00  176
  3  \w     23.00  58.00   0.50   20.00    --  -14.97  30.00  90.00   70
  4  \w     12.00  37.00   0.50   20.00    --   16.22 -61.00 150.00   50
  5  \w    -40.00  17.00   0.50   20.00    --  -14.97  30.00  90.00  114
  6  \w    -53.00   4.00   0.50   20.00    --   16.22 -61.00 150.00  114
  7  \w    -54.00   0.00   0.50   20.00    --   16.22 -30.00 150.00  108
  8  \w    -75.00 -43.00   0.50   20.00    --  -14.97 -61.00  60.00   64
  9  \w    -59.00 -20.00   0.50   20.00    --  -14.97 108.00 -11.00   78
 10  \w    -36.00  10.00   0.50   20.00    --  -14.97 -94.00 -60.00   92
 11  \w    -11.00  14.00   0.50   20.00    --   16.22 -45.00 -60.00   50
 12  \w      3.00  61.00   0.50   20.00    --   16.22-108.00-109.00  116
 13  \w    -44.00 -18.00   0.50   20.00    --   16.22 -45.00 -60.00   52
 14  \w     47.00  72.00   0.50   20.00    --   16.22  45.00-150.00   50
 15  \w     -8.00  74.00   0.50   20.00    --   16.22  77.00-150.00  164
 16  \w    -61.00 -36.00   0.50   20.00    --  -14.97 125.00-120.00   50
 17  \w    -56.00 -31.00   0.50   20.00    --  -14.97 125.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150325000
_diffrn_orient_matrix_UB_12      0.0141409000
_diffrn_orient_matrix_UB_13      -0.0463516000
_diffrn_orient_matrix_UB_21      0.0107353000
_diffrn_orient_matrix_UB_22      -0.0249097000
_diffrn_orient_matrix_UB_23      -0.0256357000
_diffrn_orient_matrix_UB_31      -0.0699037000
_diffrn_orient_matrix_UB_32      -0.0068426000
_diffrn_orient_matrix_UB_33      -0.0025493000
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0377P)^2^+0.9113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5014
_reflns_number_total             5855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01000g2.cif
_cod_data_source_block           compound1
_cod_database_code               7713434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O P V Sb Cl'
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.622
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C2(H2), C3(H3), C12(H12), C11(H11), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C14(H14A,
 H14B,H14C)
;
_shelx_res_checksum              47563
_shelx_hkl_checksum              87844
_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 4.998
_oxdiff_exptl_absorpt_empirical_full_min 0.259