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_4128009
_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 H25 Cu2 F6 N4 O2, C32 H12 B F24'
_chemical_formula_sum            'C68 H37 B Cu2 F30 N4 O2'
_chemical_formula_weight         1649.90
_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             2019-03-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.584(2)
_cell_angle_beta                 97.674(2)
_cell_angle_gamma                91.056(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8267(6)
_cell_length_b                   16.7290(9)
_cell_length_c                   18.0934(9)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.059
_cell_measurement_theta_min      2.958
_cell_volume                     3750.7(3)
_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 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  0.0385
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            119608
_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         27.147
_diffrn_reflns_theta_min         2.878
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.0943
_exptl_absorpt_correction_T_min  0.0627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0599 before and 0.0499 after correction. The Ratio of minimum to maximum transmission is 0.6649. 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    1.461
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         16565
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0524P)^2^+2.4170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13731
_reflns_number_total             16565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03635_si_002.cif
_cod_data_source_block           Zhang2157
_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               4128009
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.717
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F5B-C36 = F5-C36 = F6-C36 = F6B-C36 = F4-C36 = F4B-C36
 1.3 with sigma of 0.02
 F5B-F4B
 2.1 with sigma of 0.02
 F4B-F6B
 2.1 with sigma of 0.02
 F5B-F6B
 2.1 with sigma of 0.02
 F4-F5
 2.1 with sigma of 0.02
 F5-F6
 2.1 with sigma of 0.02
 F6-F4
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5B) = Uanis(F5)
Uanis(C60) = Uanis(C60B)
4. Rigid body (RIGU) restrains
 C68, F28, F29, F30, F28B, F29B, F30B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C36, F4, F5, F6, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, F22, F23, F24, C60, F22B, F23B, F24B, C60B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F28B)=Sof(F29B)=Sof(F30B)=1-FVAR(1)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=Sof(C60B)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=Sof(C60)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C23(H23)
6.b 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), C30(H30), C32(H32), C34(H34), 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              50043
_shelx_hkl_checksum              16525
_shelx_fab_checksum              59145
_olex2_submission_special_instructions 'No special instructions were received'