Cu site differentiation in tetracopper(i) sulfide clusters enables biomimetic N<sub>2</sub>O reduction.
Alayoglu, Pinar; Rathnayaka, Suresh C.; Chang, Tieyan; Wang, SuYin Grass; Chen, Yu-Sheng; Mankad, Neal P.; Chemical science 15 (2024) 13668–13675; doi:10.1039/d4sc00701h

data_1572467
_publ_section_title
;
 Cu site differentiation in tetracopper(i) sulfide clusters enables
 biomimetic N<sub>2</sub>O reduction.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              13668
_journal_page_last               13675
_journal_paper_doi               10.1039/d4sc00701h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C55 H54 Cu2 N4 O P4, 2(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C61 H66 Cu2 F12 N4 O3 P6'
_chemical_formula_weight         1444.07
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2024-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.148(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.668(4)
_cell_length_b                   47.890(16)
_cell_length_c                   11.500(5)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    77.15
_cell_measurement_theta_max      16.51
_cell_measurement_theta_min      2.21
_cell_volume                     6400(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      77.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            138217
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        14.070
_diffrn_reflns_theta_max         14.070
_diffrn_reflns_theta_min         0.989
_diffrn_source_current           103.0
_diffrn_source_power             103.0
_diffrn_source_voltage           1000.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9069
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.9069.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.074(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         10615
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0647P)^2^+5.2533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9320
_reflns_number_total             10615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00701h8.cif
_cod_data_source_block           s7_0m_a
_cod_database_code               1572467
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F6, F20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F6 \\sim F20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(F6) \\sim Ueq, Uanis(F20) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: F00O(0.5) F01R(0.5) F3(0.5) F6(0.5) F20(0.5) F69(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N00G(H00G), N00K(H00K), C014(H014), C017(H017), C01M(H01M)
5.b Idealised Me refined as rotating group:
 C022(H02A,H02B,H02C), C02B(H02H,H02I,H02J), C02C(H02T,H02U,H02V), C02D(H02K,
 H02L,H02M), C02E(H02W,H02X,H02Y), C02F(H02N,H02O,H02P), C02G(H02Q,H02R,H02S)
;
_olex2_submission_special_instructions 'No special instructions were received'