Reactivity of a Stable Copper-Dioxygen Complex
Betley, Theodore; Iovan, Diana A.; Wrobel, Alexandra T.; McClelland, Arthur A.; Scharf, Austin B.; Edouard, Guy A.; Chem. Commun.  (2017) –; doi:10.1039/C7CC05014C

data_7120599
_publ_section_title
;
 Reactivity of a Stable Copper-Dioxygen Complex
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05014C
_journal_year                    2017
_chemical_formula_moiety         'C66 H49 Cu N2 O2, 2(C6 H6)'
_chemical_formula_sum            'C78 H61 Cu N2 O2'
_chemical_formula_weight         1121.82
_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
_audit_creation_date             2017-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                96.0060(10)
_cell_angle_beta                 105.6810(10)
_cell_angle_gamma                104.7430(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4948(7)
_cell_length_b                   14.4326(8)
_cell_length_c                   18.0433(10)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.39
_cell_volume                     2976.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT-2014 (sHELDRICK, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44233
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.147
_diffrn_reflns_theta_max         25.112
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0467 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.9542.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink-green
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.379
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.044
_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     751
_refine_ls_number_reflns         10626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0298P)^2^+1.8198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9097
_reflns_number_total             10626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05014c2.cif
_cod_data_source_block           LCuO2
_cod_database_code               7120599
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00E(H00E), C00I(H00I), C00M(H00M), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C018(H018), C019(H019), C01A(H01A),
 C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G),
 C01H(H01H), C01I(H01I), C01J(H01J), C01L(H01N), C01M(H01O), C01N(H01P),
 C01O(H01Q), C01P(H01R), C01Q(H01S), C01R(H01T), C01S(H01U), C01V(H01Z),
 C01W(H01), C01X(H0AA), C01Y(H1AA), C01Z(H2AA), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B)
2.b Idealised Me refined as rotating group:
 C01K(H01K,H01L,H01M), C01T(H01V,H01W,H01X), C01U(H01Y,H,HA)
;
_shelx_res_checksum              42047
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'