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_4128008
_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
'C39.22 H34.43 Cu2 N4 O2.74, 2(C32 H12 B F24), 0.26(C H2 Cl2)'
_chemical_formula_sum            'C103.49 H58.97 B2 Cl0.51 Cu2 F48 N4 O2.74'
_chemical_formula_weight         2481.12
_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             2019-03-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.008(2)
_cell_angle_beta                 93.058(2)
_cell_angle_gamma                93.513(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7591(8)
_cell_length_b                   18.1984(11)
_cell_length_c                   24.8985(14)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.404
_cell_measurement_theta_min      2.785
_cell_volume                     5761.0(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Photon II MoTRIUMPH'
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            213319
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         2.806
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0711 before and 0.0565 after correction. The Ratio of minimum to maximum transmission is 0.8737. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Light Yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       Block
_exptl_crystal_F_000             2477
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1860
_refine_ls_number_reflns         21071
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0508P)^2^+8.2963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15376
_reflns_number_total             21071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03635_si_005.cif
_cod_data_source_block           Py4DMBCu_PhCCH_BArF2_Zhang2158
_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_modifier' value 'Light' changed to 'light'
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 'Yellow' changed to 'yellow'
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               4128008
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1S-C1S = Cl2S-C1S
 1.8 with sigma of 0.02
 C39-C40 = C38-C39 = C38-C37
 1.54 with sigma of 0.02
 O3-C37 = O3-C40
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F48) = Uanis(F46B)
Uanis(C71) = Uanis(C71B)
Uanis(Cl2S) = Uanis(C1S)
4. Rigid body (RIGU) restrains
 C79, F28, F29, F30, F28B, F29B, F30B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C80, F25, F26, F27, F25B, F26B, F27B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C103, F43, F44, F45, F43B, F44B, F45B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C104, F46, F47, F48, F46B, F47B, F48B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C72, F22, F23, F24, F22B, F23B, F24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F19, F20, F21, C71, F19B, F20B, F21B, C71B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C47, F1, F2, F3, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C63, F13, F14, F15, F13B, F14B, F15B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C64, F16, F17, F18, F16B, F17B, F18B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10, F11, F12, C56, F10B, F11B, F12B, C56B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C87, F31, F32, F33, F31B, F32B, F33B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C88, F34, F35, F36, F34B, F35B, F36B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C96, F40, F41, F42, F40B, F41B, F42B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C37, C38, C39, C40, Cl1S, Cl2S, C1S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cl1S, Cl2S, C1S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=Sof(C71B)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(C71)=FVAR(2)
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(3)
 Sof(F31B)=Sof(F32B)=Sof(F33B)=1-FVAR(4)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(4)
 Sof(F34B)=Sof(F35B)=Sof(F36B)=1-FVAR(5)
 Sof(F34)=Sof(F35)=Sof(F36)=FVAR(5)
 Sof(F40B)=Sof(F41B)=Sof(F42B)=1-FVAR(6)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(6)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(7)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(7)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(8)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(8)
 Sof(F43B)=Sof(F44B)=Sof(F45B)=1-FVAR(9)
 Sof(F43)=Sof(F44)=Sof(F45)=FVAR(9)
 Sof(F28B)=Sof(F29B)=Sof(F30B)=1-FVAR(10)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(10)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=Sof(C56B)=1-FVAR(11)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C56)=FVAR(11)
 Sof(F25B)=Sof(F26B)=Sof(F27B)=1-FVAR(12)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(12)
 Sof(F46B)=Sof(F47B)=Sof(F48B)=1-FVAR(13)
 Sof(F46)=Sof(F47)=Sof(F48)=FVAR(13)
 Sof(Cl1S)=Sof(Cl2S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=1-FVAR(14)
 Sof(O3)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=FVAR(14)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C14(H14), C26(H26)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C1S(H1SA,H1SB)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C42(H42), C44(H44), C46(H46), C50(H50), C52(H52), C54(H54), C58(H58),
  C60(H60), C62(H62), C66(H66), C68(H68), C70(H70), C74(H74), C76(H76),
 C78(H78), C82(H82), C84(H84), C86(H86), C90(H90), C92(H92), C94(H94), C98(H98),
  C100(H100), C102(H102)
;
_shelx_res_checksum              53451
_shelx_hkl_checksum              906
_shelx_fab_checksum              61047
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'