Dicopper μ-Oxo, μ-Nitrosyl Complex from the Activation of NO or Nitrite at a Dicopper Center.
Tao, Wenjie; Bower, Jamey K.; Moore, Curtis E.; Zhang, Shiyu; Journal of the American Chemical Society 141 (2019) 10159–10164; doi:10.1021/jacs.9b03635

data_4128011
_publ_section_title
;
 Dicopper \m-Oxo, \m-Nitrosyl Complex from the Activation of NO or Nitrite
 at a Dicopper Center.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10159
_journal_page_last               10164
_journal_paper_doi               10.1021/jacs.9b03635
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C31 H28 Cu2 N5 O5, C4 H6 F3 O4 S, C F3 O3 S'
_chemical_formula_sum            'C36 H34 Cu2 F6 N5 O12 S2'
_chemical_formula_weight         1033.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.398(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.132(4)
_cell_length_b                   10.4087(10)
_cell_length_c                   14.2824(15)
_cell_measurement_reflns_used    5071
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.291
_cell_measurement_theta_min      2.861
_cell_volume                     4926.3(9)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9690
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         2.861
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.260242
_exptl_absorpt_correction_T_min  0.220663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 59328 reflections, Rint = 0.0525
 (31200 with I > 3sig(I), Rint = 0.0412)
;
_exptl_crystal_colour            Red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       Block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         9690
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+13.3702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7803
_reflns_number_total             9690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03635_si_004.cif
_cod_data_source_block           Py4DMBCu_O_NO_OTf2_WJ022819
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Red' changed to 'red'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4128011
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6807(16)
 0.3193(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{O1, N1}
4. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(N1) = Uanis(O1)
Uanis(C19) = Uanis(C17)
Uanis(N4) = Uanis(N3)
5. Rigid body (RIGU) restrains
 N3, C17, C18, C19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7, C12, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cu2, O4, N3, N4, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S2A, F4A, F5A, F6A, O4A, O5A, O6A, C2A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2S, O1S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3SB, C1S, C3S, C2S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{S1A, F1A, F2A, F3A, O1A, O2A, O3A, C1A} sigma for 1-2: 0.02, 1-3: 0.04
as
{S2A, F4A, F5A, F6A, O4A, O5A, O6A, C2A}
7. Others
 1*[Sof(C3SB)+Sof(H3SA)+Sof(H3SB)+Sof(H3SC)]+1*[Sof(C1S)+Sof(H1SA)+Sof(H1SB)+
 Sof(H1SC)]+1*[Sof(C3S)+Sof(H3SD)+Sof(H3SE)+Sof(H3SF)]=1 with esd of 0
 Sof(C3SB)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(2)
 Sof(C3S)=Sof(H3SD)=Sof(H3SE)=Sof(H3SF)=FVAR(3)
 Fixed Sof: C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5)
 H11(0.5) C12(0.5) O2(0.5) N1(0.5) O1(0.5) N3(0.5) N4(0.5) C13(0.5) H13(0.5)
 C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) C18(0.5)
 H18(0.5) C19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5)
 C23(0.5) H23(0.5) S1A(0.5) F1A(0.5) F2A(0.5) F3A(0.5) O1A(0.5) O2A(0.5)
 O3A(0.5) C1A(0.5) S2A(0.5) F4A(0.5) F5A(0.5) F6A(0.5) O4A(0.5) O5A(0.5)
 O6A(0.5) C2A(0.5) O2S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C5S(0.5)
 C6S(0.5) H6SA(0.5) H6SB(0.5) H1A(0.5)
8.a Ternary CH refined with riding coordinates:
 C6(H6), C18(H18)
8.b Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H1A), C1S(H1SA,H1SB,H1SC), C3SB(H3SA,H3SB,
 H3SC), C3S(H3SD,H3SE,H3SF)
8.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23)
8.d Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12)
;
_shelx_res_checksum              99702
_shelx_hkl_checksum              51392
_shelx_fab_checksum              26852
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'