Synthesis and Catalytic Reactivity of a Dicopper(II) μ-η(2):η(2)-Peroxo Species Supported by 1,4,7-Tri-tert-butyl-1,4,7-triazacyclononane.
Karahalis, Gregory J.; Thangavel, Arumugam; Chica, Bryant; Bacsa, John; Dyer, R. Brian; Scarborough, Christopher C.; Inorganic chemistry 55 (2016) 1102–1107; doi:10.1021/acs.inorgchem.5b02205

data_4344699
_publ_section_title
;
 Synthesis and Catalytic Reactivity of a Dicopper(II)
 \m-\h(2):\h(2)-Peroxo Species Supported by
 1,4,7-Tri-tert-butyl-1,4,7-triazacyclononane.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1102
_journal_page_last               1107
_journal_paper_doi               10.1021/acs.inorgchem.5b02205
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H78 Cu2 N6 O2, 2(C F3 O3 S)'
_chemical_formula_sum            'C38 H78 Cu2 F6 N6 O8 S2'
_chemical_formula_weight         1052.26
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2014-09-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                70.464(2)
_cell_angle_beta                 65.2057(19)
_cell_angle_gamma                60.4756(19)
_cell_formula_units_Z            1
_cell_length_a                   10.9185(16)
_cell_length_b                   10.9583(16)
_cell_length_c                   12.4586(18)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.381
_cell_measurement_theta_min      2.397
_cell_volume                     1162.0(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (Bruker, 2014)'
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34678
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1216 before and 0.0410 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1426 before and 0.0530 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.1300 before and 0.0538 after correction.
 The Ratio of minimum to maximum transmission is 0.76.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 34574 reflections, Rint = 0.0750
 (12882 with I > 3sig(I), Rint = 0.0517)
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method
;
 The material was recrystallised from a mixture of DCM and pentane by 
 slow evaporation.
;
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.635
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0795P)^2^+2.7950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3562
_reflns_number_total             4336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02205_si_001.cif
_cod_data_source_block           3-230
_cod_database_code               4344699
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.617
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C1(H1A,H1B), C5(H5A,H5B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C18(H18A,H18B,
 H18C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C8(H8A,
 H8B,H8C), C14(H14A,H14B,H14C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'