Heterodinuclear Cu(I)/Mo(VI) chemistry with bifunctional dibenzobarrelene ligands.
Chandima, A. M. Buddhika; Sgro, Griffyn; Hilditch, Sierra M.; Kaluarachchige Don, Umesh I.; Ward, Cassandra L.; Anderson, Dennis P.; Herman, Limor; Gelman, Dmitri; Lord, Richard L.; Groysman, Stanislav; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14716–14727; doi:10.1039/d5dt01337b

data_1575687
_publ_section_title
;
 Heterodinuclear Cu(I)/Mo(VI) chemistry with bifunctional dibenzobarrelene
 ligands.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14716
_journal_page_last               14727
_journal_paper_doi               10.1039/d5dt01337b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C45.705 H35.551 Cu D11.805 O3.888 P2 S1.968, C2 D6 O S, F6 P, 0.111(C2 H2 O), 1[C2H6SO]'
_chemical_formula_sum            'C49.93 H41.77 Cu D17.8 F6 O6 P3 S3.97'
_chemical_formula_weight         1171.27
_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             2025-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                77.997(2)
_cell_angle_beta                 88.205(2)
_cell_angle_gamma                70.621(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1992(8)
_cell_length_b                   13.8549(9)
_cell_length_c                   15.7166(9)
_cell_measurement_reflns_used    9263
_cell_measurement_temperature    101.00
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.44
_cell_volume                     2649.8(3)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101.00
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.8 mm pinhole collimator'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.007
_diffrn_reflns_theta_min         1.847
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1421 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8976.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1197
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.071
_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     992
_refine_ls_number_reflns         16860
_refine_ls_number_restraints     2412
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.4426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13421
_reflns_number_total             16860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01337b3.cif
_cod_data_source_block           sag68
_cod_depositor_comments
'Adding full bibliography for 1575687--1575689.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C49.93 H41.77 Cu D17.80 F6 O6 P3 S3.97'
_cod_database_code               1575687
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.899
_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, All O(H) groups
2. Shared sites
{C20, C20B}
{C21, C21B}
3. Restrained distances
 O4B-H4B = O4-H4 = O3-H3
 0.84 with sigma of 0.02
 S1-O1 \\sim S1B-O1B \\sim S2B-O2B \\sim S2-O2 \\sim S3-O5
 with sigma of 0.02
 S3-C48 \\sim S3-C47 \\sim S1-C44 \\sim S1-C43 \\sim S1B-C44B \\sim S1B-C43B
\\sim S2-C45 \\sim S2B-C45B ~
 S2B-C46B \\sim S2-C46
 with sigma of 0.02
 C45B-C46B \\sim C45-C46 \\sim C48-C47 \\sim C43-C44 \\sim C44B-C43B
 with sigma of 0.02
 C6B-C1 \\sim C6-C1 \\sim C6B-C5B \\sim C6-C5 \\sim C5B-C4B \\sim C5-C4 \\sim
C3B-C4B \\sim C4-C3 \\sim C2B-
 C3B \\sim C3-C2 \\sim C2-C1 \\sim C37-C42 \\sim C42-C41 \\sim C41-C40 \\sim
C40-C39 \\sim C39-C38 \\sim C37-
 C38 \\sim C38-C37B \\sim C40B-C41B \\sim C41B-C42B \\sim C42B-C37B \\sim
C40B-C39 \\sim C30-C29 \\sim C29-
 C28B \\sim C30-C26 \\sim C28B-C27B \\sim C28-C27 \\sim C29-C28 \\sim C26-C25
\\sim C27B-C25B \\sim C27-C25
 \\sim C26-C25B \\sim C14-C13 \\sim C14B-C13 \\sim C15B-C14B \\sim C15-C14
\\sim C18-C13 \\sim C18-C17 ~
 C18-C17B \\sim C17B-C16B \\sim C17-C16 \\sim C16B-C15B \\sim C16-C15
 with sigma of 0.02
 O3B-C21C \\sim O4-C24 \\sim O4B-C24B \\sim O3-C21 \\sim O3C-C21B
 with sigma of 0.02
 C23B-C22 \\sim C23-C22 \\sim C59-C23B \\sim C23-C20 \\sim C20-C19 \\sim
C59-C21C \\sim C59-C19B ~
 C24B-C23B \\sim C24-C23 \\sim C21B-C20B
 with sigma of 0.02
 S3-O5 \\sim S3B-O5B
 with sigma of 0.02
 S3-C47 \\sim S3B-C47B
 with sigma of 0.02
 S3-C48 \\sim S3B-C48B
 with sigma of 0.02
 O5-C47 \\sim O5B-C47B
 with sigma of 0.04
 O5-C48 \\sim O5B-C48B
 with sigma of 0.04
 C47-C48 \\sim C47B-C48B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
Uanis(C20) = Uanis(C20B)
Uanis(C21) = Uanis(C21B)
5. Others
 1*[Sof(S1)+Sof(O1)+Sof(C43)+Sof(D43A)+Sof(D43B)+Sof(D43C)+Sof(C44)+Sof(D44A)+
 Sof(D44B)+Sof(D44C)]+1*[Sof(S1B)+Sof(O1B)+Sof(C43B)+Sof(D43D)+Sof(D43E)+
 Sof(D43F)+Sof(C44B)+Sof(D44D)+Sof(D44E)+Sof(D44F)]+1*[Sof(O1W)]=1 with esd of
 0.001
 Sof(H22A)=Sof(H29A)=Sof(C59)=Sof(H59)=Sof(O3B)=Sof(H3B)=Sof(O4B)=Sof(H4B)=
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=
 Sof(C19B)=Sof(H19B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24C)=Sof(H24D)=
 Sof(C25B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C21C)=Sof(H21C)=
 Sof(H21D)=1-FVAR(1)
 Sof(O4)=Sof(H4)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(C19)=Sof(H19)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(C25)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(H29)=FVAR(1)
 Sof(H39A)=Sof(C37B)=Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=
 Sof(H42B)=1-FVAR(2)
 Sof(C37)=Sof(H38)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=
 Sof(H42)=FVAR(2)
 Sof(S2B)=Sof(O2B)=Sof(C45B)=Sof(D45D)=Sof(D45E)=Sof(D45F)=Sof(C46B)=Sof(D46D)=
 Sof(D46E)=Sof(D46F)=1-FVAR(3)
 Sof(S2)=Sof(O2)=Sof(C45)=Sof(D45A)=Sof(D45B)=Sof(D45C)=Sof(C46)=Sof(D46A)=
 Sof(D46B)=Sof(D46C)=FVAR(3)
 Sof(S1)=Sof(O1)=Sof(C43)=Sof(D43A)=Sof(D43B)=Sof(D43C)=Sof(C44)=Sof(D44A)=
 Sof(D44B)=Sof(D44C)=FVAR(4)
 Sof(C20B)=Sof(C21B)=Sof(H21E)=Sof(H21F)=Sof(O3C)=0.813*(1-FVAR(6))
 Sof(O3)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21A)=Sof(H21B)=0.813*FVAR(6)
 Sof(H3)=FVAR(5)
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3BA)=Sof(C4B)=Sof(H4BA)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(H6B)=1-FVAR(6)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(C4)=Sof(H4A)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(6)
 Sof(S1B)=Sof(O1B)=Sof(C43B)=Sof(D43D)=Sof(D43E)=Sof(D43F)=Sof(C44B)=Sof(D44D)=
 Sof(D44E)=Sof(D44F)=FVAR(7)
 Sof(F1B)=Sof(F2B)=Sof(F4B)=Sof(F6B)=1-FVAR(9)
 Sof(F1)=Sof(F2)=Sof(F4)=Sof(F6)=FVAR(9)
 Sof(S3B)=Sof(O5B)=Sof(C47B)=Sof(D47D)=Sof(D47E)=Sof(D47F)=Sof(C48B)=Sof(D48D)=
 Sof(D48E)=Sof(D48F)=1-FVAR(10)
 Sof(S3)=Sof(O5)=Sof(C47)=Sof(D47A)=Sof(D47B)=Sof(D47C)=Sof(C48)=Sof(D48A)=
 Sof(D48B)=Sof(D48C)=FVAR(10)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C22(H22), C22(H22A), C23(H23), C59(H59), C19B(H19B),
 C23B(H23B)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C24(H24A,H24B), C21B(H21E,H21F), C24B(H24C,H24D), C21C(H21C,
 H21D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4A), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C27(H27), C28(H28), C29(H29),
 C29(H29A), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
 C39(H39), C39(H39A), C40(H40), C41(H41), C42(H42), C2B(H2B), C3B(H3BA),
 C4B(H4BA), C5B(H5B), C6B(H6B), C14B(H14B), C15B(H15B), C16B(H16B), C27B(H27B),
 C28B(H28B), C40B(H40B), C41B(H41B), C42B(H42B)
6.d Tetrahedral OH refined with riding coordinates:
 O3B(H3B)
6.e Idealised Me refined as rotating group:
 C43(D43A,D43B,D43C), C44(D44A,D44B,D44C), C45(D45A,D45B,D45C), C46(D46A,D46B,
 D46C), C47(D47A,D47B,D47C), C48(D48A,D48B,D48C), C43B(D43D,D43E,D43F),
 C44B(D44D,D44E,D44F), C45B(D45D,D45E,D45F), C46B(D46D,D46E,D46F), C47B(D47D,
 D47E,D47F), C48B(D48D,D48E,D48F)
6.f Idealised tetrahedral OH refined as rotating group:
 O4(H4), O4B(H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57373
_shelx_fab_checksum              59836
_olex2_submission_special_instructions 'No special instructions were received'