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_4128010
_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
'C36 H38 Cu2 N5 O6, 2(C32 H12 B F24), 2(C4 H8 O)'
_chemical_formula_sum            'C108 H78 B2 Cu2 F48 N5 O8'
_chemical_formula_weight         2634.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                61.744(3)
_cell_angle_beta                 77.290(4)
_cell_angle_gamma                85.224(4)
_cell_formula_units_Z            1
_cell_length_a                   12.6825(15)
_cell_length_b                   17.1535(19)
_cell_length_c                   17.278(2)
_cell_measurement_reflns_used    7862
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.247
_cell_measurement_theta_min      2.773
_cell_volume                     3228.8(7)
_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      150
_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 0.985
_diffrn_measured_fraction_theta_max 0.984
_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_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21423
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_min         2.888
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0686
_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 107496 reflections, Rint = 0.1081
 (32337 with I > 3sig(I), Rint = 0.0584)
;
_exptl_crystal_colour            Red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       Block
_exptl_crystal_F_000             1325
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.057(5)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         11664
_refine_ls_number_restraints     792
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.1087
_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^)+(0.1231P)^2^+8.3791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2789
_refine_ls_wR_factor_ref         0.3026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7024
_reflns_number_total             11664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03635_si_003.cif
_cod_data_source_block           Py4DMBCu_O_NO_BArF2_Zhang2320
_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_original_cell_volume        3228.9(7)
_cod_database_code               4128010
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F10-C52 = F12-C52 = F11-C52
 1.3 with sigma of 0.02
 F10B-C52B = F12B-C52B = F11B-C52B
 1.3 with sigma of 0.02
 F12-F11
 2.1 with sigma of 0.02
 F11-F10
 2.1 with sigma of 0.02
 F10-F12
 2.1 with sigma of 0.02
 F10B-F12B
 2.1 with sigma of 0.02
 F12B-F11B
 2.1 with sigma of 0.02
 F10B-F11B
 2.1 with sigma of 0.02
 F15B-C59 = F14-C59 = F14B-C59 = F13-C59 = F13B-C59 = F15-C59
 1.3 with sigma of 0.02
 F14-F13
 2.1 with sigma of 0.02
 F13-F15
 2.1 with sigma of 0.02
 F14-F15
 2.1 with sigma of 0.02
 F14B-F13B
 2.1 with sigma of 0.02
 F13B-F15B
 2.1 with sigma of 0.02
 F15B-F14B
 2.1 with sigma of 0.02
 F6-C44 = F6B-C44 = F5-C44 = F5B-C44 = F4-C44 = F4B-C44
 1.3 with sigma of 0.02
 F6-F5
 2.1 with sigma of 0.02
 F6-F4
 2.1 with sigma of 0.02
 F4-F5
 2.1 with sigma of 0.02
 F6B-F5B
 2.1 with sigma of 0.02
 F6B-F4B
 2.1 with sigma of 0.02
 F4B-F5B
 2.1 with sigma of 0.02
 F19B-C67 = F21-C67 = F21B-C67 = F20B-C67 = F19-C67 = F20-C67
 1.3 with sigma of 0.02
 F19B-F21B
 2.1 with sigma of 0.02
 F21B-F20B
 2.1 with sigma of 0.02
 F20B-F19B
 2.1 with sigma of 0.02
 F21-F20
 2.1 with sigma of 0.02
 F20-F19
 2.1 with sigma of 0.02
 F19-F21
 2.1 with sigma of 0.02
 F17-C60 = F17B-C60 = F18-C60 = F18B-C60 = F16-C60 = F16B-C60
 1.3 with sigma of 0.02
 F17B-F18B
 2.1 with sigma of 0.02
 F18B-F16B
 2.1 with sigma of 0.02
 F16B-F17B
 2.1 with sigma of 0.02
 F17-F16
 2.1 with sigma of 0.02
 F16-F18
 2.1 with sigma of 0.02
 F18-F17
 2.1 with sigma of 0.02
 C52B-C49 = C52-C49
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O6B)
Uanis(C52B) = Uanis(C52)
Uanis(C52B) = Uanis(C52) = Uanis(C49)
Uanis(F11B) = Uanis(F11)
4. Rigid body (RIGU) restrains
 C41, C44, C49, C55, C57, C59, C60, C63, C65, C67, C68, F4, F5, F6, F10, F11,
 F12, F13, F14, F15, F16, F17, F18, F19, F20, F21, F22, F23, F24, C52, F4B, F5B,
  F6B, F10B, F11B, F12B, F13B, F14B, F15B, F16B, F17B, F18B, F19B, F20B, F21B,
 F22B, F23B, F24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, C29, C30, C31, C32, C33, C34, C35, C36, O1S, C1S, C2S, C3S, C4S, O2S,
 C5S, C6S, C7S, C8S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, O3, N2, N3, N4, N5, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12,
 C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, F10, F11, F12, C52, F10B, F11B, F12B, C52B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(O6)]+1*[Sof(O6B)]=0.5 with esd of 0
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(4)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(4)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(5)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(5)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(6)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(6)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(7)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(7)
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(8)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(8)
 Sof(C52B)=1-FVAR(9)
 Sof(C52)=FVAR(9)
 Fixed Sof: Cu1(0.5) Cu2(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) N1(0.5)
 N2(0.5) N3(0.5) N4(0.5) N5(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5)
 H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) 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) 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) H19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5)
 C23(0.5) H23(0.5) C24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29A(0.5) H29B(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
 O2S(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) C7S(0.5)
 H7SA(0.5) H7SB(0.5) C8S(0.5) H8SA(0.5) H8SB(0.5)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C1S(H1SA,H1SB),
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB),
  C7S(H7SA,H7SB), C8S(H8SA,H8SB)
6.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), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25),
  C26(H26), C27(H27), C28(H28), C38(H38), C40(H40), C42(H42), C46(H46),
 C48(H48), C50(H50), C54(H54), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66)
;
_shelx_res_checksum              44591
_shelx_hkl_checksum              67508
_shelx_fab_checksum              19569
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'