A trans-Hyponitrite Intermediate in the Reductive Coupling and Deoxygenation of Nitric Oxide by a Tricopper-Lewis Acid Complex.
Lionetti, Davide; de Ruiter, Graham; Agapie, Theodor; Journal of the American Chemical Society 138 (2016) 5008–5011; doi:10.1021/jacs.6b01083

data_4130169
_publ_section_title
;
 A trans-Hyponitrite Intermediate in the Reductive Coupling and
 Deoxygenation of Nitric Oxide by a Tricopper-Lewis Acid Complex.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5008
_journal_page_last               5011
_journal_paper_doi               10.1021/jacs.6b01083
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C146 H156 Cu6 N32 O8 Y2, 2(C4 H10 O), 6(C F3 O3 S), 0.5(C4 H6 N2)'
_chemical_formula_sum            'C162 H179 Cu6 F18 N33 O28 S6 Y2'
_chemical_formula_weight         4129.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                105.556(3)
_cell_angle_beta                 105.602(3)
_cell_angle_gamma                94.915(3)
_cell_formula_units_Z            1
_cell_length_a                   13.8507(13)
_cell_length_b                   16.8194(17)
_cell_length_c                   21.214(2)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.45
_cell_volume                     4518.8(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type
;   
'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS' 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            238176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0694 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.9327. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         20712
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0847P)^2^+9.8296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15785
_reflns_number_total             20712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01083_si_001.cif
_cod_data_source_block           p15262_a
_cod_original_cell_volume        4518.7(8)
_cod_database_code               4130169
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N16, C83}
3. Restrained distances
 O17-C79 \\sim O17-C80
 with sigma of 0.02
 C79-C78 \\sim C80-C81
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(N16) = Uiso(C83)
5. Others
 Sof(S3)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(O11)=Sof(O13)=Sof(O15)=Sof(C76)=1-FVAR(1)
 Sof(S4)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(O12)=Sof(O14)=Sof(O16)=Sof(C77)=FVAR(1)
 Fixed Sof: N16(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C36(H36A,H36B), C37(H37A,H37B),
  C43(H43A,H43B), C59(H59A,H59B), C60(H60A,H60B), C66(H66A,H66B), C79(H79A,
 H79B), C80(H80A,H80B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C32(H32), C39(H39), C40(H40),
  C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51),
 C53(H53), C55(H55), C62(H62), C63(H63), C64(H64), C65(H65), C68(H68), C69(H69),
  C70(H70), C71(H71)
6.c Idealised Me refined with riding coordinates:
 C78(H78A,H78B,H78C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C35(H35A,H35B,H35C), C50(H50A,H50B,H50C), C58(H58A,H58B,
 H58C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              21727
_shelx_hkl_checksum              2756
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'