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_1575688
_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
'C47.463 H43.435 Cu N O5.12 P2, F6 P, 1.634(C4 H8 O), 0.5(C4 H10 O)'
_chemical_formula_sum            'C56 H61.51 Cu F6 N O7.26 P3'
_chemical_formula_weight         1135.10
_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             2024-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                74.360(4)
_cell_angle_beta                 84.718(4)
_cell_angle_gamma                74.392(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7377(16)
_cell_length_b                   14.6834(18)
_cell_length_c                   15.876(2)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.155
_cell_measurement_theta_min      2.498
_cell_volume                     2753.3(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.1756
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11314
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.482
_diffrn_reflns_theta_min         2.094
_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
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.745374
_exptl_absorpt_correction_T_min  0.281561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1610 before and 0.0957 after correction.
 
For component 2:
 wR2(int) was 0.1959 before and 0.1099 after correction.
 The Ratio of minimum to maximum transmission is 0.38.

Final HKLF 4 output contains 288649 reflections, Rint = 0.1767
 (43100 with I > 3sig(I), Rint = 0.0722)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       prism
_exptl_crystal_F_000             1181
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.615
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         11314
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1392P)^2^+2.7174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7904
_reflns_number_total             11314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01337b3.cif
_cod_data_source_block           mo_sg33_0m_4
_cod_depositor_comments
'Adding full bibliography for 1575687--1575689.cif.'
_cod_database_code               1575688
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.921
_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,H) groups
2. Restrained distances
 O1SB-C4SB = O1SB-C1SB
 1.44 with sigma of 0.02
 C4SB-C3SB = C2SB-C1SB
 1.53 with sigma of 0.02
 C3SB-C2SB
 1.54 with sigma of 0.02
 O1SB-C3SB = O1SB-C2SB = C4SB-C2SB = C3SB-C1SB
 2.38 with sigma of 0.04
 C1E-C2E \\sim C3E-C4E
 with sigma of 0.02
 O1E-C2E \\sim O1E-C3E
 with sigma of 0.02
 C1E-O1E \\sim C4E-O1E
 with sigma of 0.02
 O1SB-C4SB \\sim O1SB-C1SB \\sim O1S-C1S \\sim O1S-C4S \\sim O1SA-C1SA \\sim
O1SA-C4SA
 with sigma of 0.01
 C1SB-C2SB \\sim C4SB-C3SB \\sim C2S-C1S \\sim C4S-C3S \\sim C3S-C2S \\sim
C3SA-C4SA \\sim C2SA-C3SA ~
 C2SA-C1SA \\sim C2SB-C3SB
 with sigma of 0.01
 C4SA-C1SA \\sim C4SB-C1SB \\sim C1S-C4S
 with sigma of 0.01
 C3S-O1S \\sim C2SA-O1SA \\sim C2S-O1S \\sim C3SA-O1SA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.002 within 2A
Cu1 \\sim O1S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim O1SA \\sim O1W
\\sim C1SA \\sim C2SA \\sim C3SA \\sim C4SA \\sim O1SB \\sim C1SB \\sim C2SB
\\sim C3SB \\sim C4SB: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.002 within 2A
4. Others
 Sof(O1SB)=Sof(C1SB)=Sof(H1SA)=Sof(H1SB)=Sof(C2SB)=Sof(H2SA)=Sof(H2SB)=
 Sof(C3SB)=Sof(H3SA)=Sof(H3SB)=Sof(C4SB)=Sof(H4SA)=Sof(H4SB)=1-FVAR(1)
 Sof(O1SA)=Sof(C1SA)=Sof(H1SE)=Sof(H1SF)=Sof(C2SA)=Sof(H2SE)=Sof(H2SF)=
 Sof(C3SA)=Sof(H3SE)=Sof(H3SF)=Sof(C4SA)=Sof(H4SE)=Sof(H4SF)=FVAR(1)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(2)
 Fixed Sof: O1E(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) H1EC(0.5) C2E(0.5) H2EA(0.5)
 H2EB(0.5) C3E(0.5) H3EA(0.5) H3EB(0.5) C4E(0.5) H4EA(0.5) H4EB(0.5) H4EC(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C27(H27), C30(H30)
5.c Secondary CH2 refined with riding coordinates:
 C1S(H1SC,H1SD), C2S(H2SC,H2SD), C3S(H3SC,H3SD), C4S(H4SC,H4SD), C1SA(H1SE,
 H1SF), C2SA(H2SE,H2SF), C3SA(H3SE,H3SF), C4SA(H4SE,H4SF), C1SB(H1SA,H1SB),
 C2SB(H2SA,H2SB), C3SB(H3SA,H3SB), C4SB(H4SA,H4SB), C2E(H2EA,H2EB), C3E(H3EA,
 H3EB)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C23(H23), C24(H24), C25(H25), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44)
5.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C46(H46A,H46B,H46C), C1E(H1EA,H1EB,
 H1EC), C4E(H4EA,H4EB,H4EC)
;
_shelx_res_checksum              15259
_olex2_submission_special_instructions 'No special instructions were received'