Solubilizing dimolybdenum paddlewheel complexes for energy storage applications.
Gersib, Simon G.; Subasinghe, S. M. Supundrika; Mankad, Neal P.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10546–10548; doi:10.1039/d5dt01246e

data_7718962
_publ_section_title
;
 Solubilizing dimolybdenum paddlewheel complexes for energy storage
 applications.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10546
_journal_page_last               10548
_journal_paper_doi               10.1039/d5dt01246e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H47 B2 F8 Li2 Mo2 N4 O12, 0.5[C4H8O]'
_chemical_formula_sum            'C42 H51 B2 F8 Li2 Mo2 N4 O12.5'
_chemical_formula_weight         1191.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-29 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.854(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.679(11)
_cell_length_b                   11.018(2)
_cell_length_c                   18.843(4)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.83
_cell_volume                     9886(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58580
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.341
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'sealed tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0412 before and 0.0362 after correction.
The Ratio of minimum to maximum transmission is 0.9254.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         10058
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+28.7363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9397
_reflns_number_total             10058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01246e2.cif
_cod_data_source_block           sg7_0m
_cod_depositor_comments
'Adding full bibliography for 7718960--7718962.cif.'
_cod_original_formula_sum        'C42 H51 B2 F8 Li2 Mo2 N4 O12.50'
_cod_database_code               7718962
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.012
_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
 F00A-B01R \\sim F00B-B01S
 with sigma of 0.02
 F00A-Li \\sim F00B-Li
 with sigma of 0.02
 F00U-B01R \\sim F00V-B01S
 with sigma of 0.02
 F00U-Li1 \\sim F00V-Li1
 with sigma of 0.02
 B01R-F1 \\sim B01S-F1A
 with sigma of 0.02
 B01R-F2 \\sim B01S-F2A
 with sigma of 0.02
 F00A-F00U \\sim F00B-F00V
 with sigma of 0.04
 F00A-F1 \\sim F00B-F1A
 with sigma of 0.04
 F00A-F2 \\sim F00B-F2A
 with sigma of 0.04
 F00U-F1 \\sim F00V-F1A
 with sigma of 0.04
 F00U-F2 \\sim F00V-F2A
 with sigma of 0.04
 B01R-Li1 \\sim B01S-Li1
 with sigma of 0.04
 B01R-Li \\sim B01S-Li
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
3. Others
 Sof(F00V)=Sof(B01S)=Sof(F1A)=Sof(F2A)=Sof(F00B)=1-FVAR(1)
 Sof(F00A)=Sof(F00U)=Sof(B01R)=Sof(F1)=Sof(F2)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C016(H01a,H01b), C01G(H01i,H01j), C01H(H01k,H01l), C01I(H01m,H01n), C01N(H01t,
 H01u)
4.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00Y(H00Y), C00Z(H00Z),
 C011(H011), C012(H012), C013(H013), C014(H014), C018(H018), C019(H019),
 C01C(H01f), C01D(H01g), C01E(H01h), C01J(H01o), C01M(H01s), C01O(H01v),
 C01S(H01w)
4.c Idealised Me refined as rotating group:
 C01A(H01c,H01d,H01e), C01K(H01p,H01q,H01r), C01T(H01x,H01y,H), C01W(H01z,Ha,
 Hb), C01X(H01,Hc,Hd), C01Y(H1,He,Hf)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 136 electrons were 
found in a volume of 672\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C4H8O] per formula unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27516
_shelx_hkl_checksum              31705
_shelx_fab_checksum              28958
_olex2_submission_special_instructions 'No special instructions were received'