Unusually air-stable copper(i) complexes showing high selectivity for carbon monoxide.
Saeednia, Borna; Sragow, Aria M.; Lin, Yannan; Sheehan, Colton J.; Metlay, Amy S.; Gau, Michael R.; Dye, Samantha A.; O'Konski, Sarah P; Mallouk, Thomas E.; Dmochowski, Ivan J.; Chemical science 16 (2025) 5058–5063; doi:10.1039/d5sc00237k

data_1573942
_publ_section_title
;
 Unusually air-stable copper(i) complexes showing high selectivity for
 carbon monoxide.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              5058
_journal_page_last               5063
_journal_paper_doi               10.1039/d5sc00237k
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C51 H54 Cu N7 O6, C F3 O3 S, C4 H7 N'
_chemical_formula_sum            'C56 H61 Cu F3 N8 O9 S'
_chemical_formula_weight         1142.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-05-29 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.111(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0509(4)
_cell_length_b                   16.2265(2)
_cell_length_c                   20.4026(5)
_cell_measurement_reflns_used    43652
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4810
_cell_measurement_theta_min      2.4280
_cell_volume                     5411.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Dectris Pilatus3 R 200K'
_diffrn_measured_fraction_theta_full 0.999
_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    -73.00  17.00   0.50   15.50    --    5.07 -37.00   0.00  180
  2  \w     -9.00  24.00   0.50   15.50    --   -5.38 -99.00   0.00   66
  3  \w     39.00  84.00   0.50   15.50    --    5.07-178.00   0.00   90
  4  \w    -23.00   2.00   0.50   15.50    --   -5.38 -99.00 -60.00   50
  5  \w     39.00  84.00   0.50   15.50    --    5.07-178.00 -30.00   90
  6  \w     40.00  66.00   0.50   15.50    --    5.07-178.00-120.00   52
  7  \w     56.00  81.00   0.50   15.50    --    5.07-178.00-150.00   50
  8  \w    -71.00  16.00   0.50   15.50    --   -5.38 -77.00   0.00  174
  9  \w    -85.00   5.00   0.50   15.50    --   -5.38 -19.00-180.00  180
 10  \w    -83.00   9.00   0.50   15.50    --   -5.38 -37.00  90.00  184
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0414026000
_diffrn_orient_matrix_UB_12      0.0101644000
_diffrn_orient_matrix_UB_13      -0.0089792000
_diffrn_orient_matrix_UB_21      -0.0097178000
_diffrn_orient_matrix_UB_22      -0.0059126000
_diffrn_orient_matrix_UB_23      -0.0372060000
_diffrn_orient_matrix_UB_31      -0.0086427000
_diffrn_orient_matrix_UB_32      -0.0420923000
_diffrn_orient_matrix_UB_33      0.0030660000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            101561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       needle
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         12400
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0381P)^2^+6.6067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10938
_reflns_number_total             12400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00237k2.cif
_cod_data_source_block           9752_CuL1N3_OTf2
_cod_depositor_comments
'Adding full bibliography for 1573940--1573942.cif.'
_cod_database_code               1573942
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N8 \\sim N8* \\sim C53 \\sim C53* \\sim C54 \\sim C54*: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: N8(0.65) N8*(0.35) C53(0.65) C53*(0.35) C54(0.65) H54(0.65) C54*
 (0.35) H54*(0.35) H55A(0.65) H55B(0.65) H55C(0.65) H55D(0.35) H55E(0.35)
 H55F(0.35) H56A(0.65) H56B(0.65) H56C(0.65) H56D(0.35) H56E(0.35) H56F(0.35)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C54(H54), C54*(H54*)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C15(H15A,H15B), C16(H16A,H16B), C30(H30A,H30B), C31(H31A,H31B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14), C19(H19), C22(H22),
 C25(H25), C26(H26), C28(H28), C29(H29), C34(H34), C37(H37), C40(H40), C41(H41),
  C43(H43), C44(H44)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C23(H23A,H23B,H23C), C38(H38A,H38B,H38C), C55(H55A,H55B,
 H55C), C55(H55D,H55E,H55F), C56(H56A,H56B,H56C), C56(H56D,H56E,H56F)
;
_shelx_res_checksum              31129
_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 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.700