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_7713435
_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         'C66 H102 Cu2 N2 O20 P4 Sb4, 2(C H4 O)'
_chemical_formula_sum            'C68 H110 Cu2 N2 O22 P4 Sb4'
_chemical_formula_weight         2045.53
_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
_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                99.588(2)
_cell_angle_beta                 93.106(2)
_cell_angle_gamma                114.547(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8207(14)
_cell_length_b                   13.3637(15)
_cell_length_c                   13.7013(15)
_cell_measurement_reflns_used    8726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.33
_cell_volume                     2085.5(4)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16745
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         1.522
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0473 before and 0.0212 after correction.
The Ratio of minimum to maximum transmission is 0.7487.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0358P)^2^+1.9129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             8416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01000g2.cif
_cod_data_source_block           compound5
_cod_database_code               7713435
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.666
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C27(H27), C25(H25), C26(H26), C15(H15), C24(H24), C5(H5), C2(H2),
 C6(H6), C12(H12), C11(H11), C3(H3), C14(H14)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C21(H21A,H21B,
 H21C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C34(H34A,
 H34B,H34C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17352
_shelx_hkl_checksum              48750
_olex2_submission_special_instructions 'No special instructions were received'