Mono-and Tetra-nuclear copper complexes bearing bis(imino)phenoxide derived ligands: catalytic evaluation for benzene oxidation and ROP of epsilon-caprolactone
Wang, Xue; Zhao, Keqing; Elsegood, Mark Robert James; Prior, Timothy J.; Liu, Xiaoming; Li, Wu; Sanz, Sergio; Brechin, Euan K.; Redshaw, Carl; RSC Adv.  (2015) –; doi:10.1039/C5RA08696E

data_7220720
_publ_section_title
;
 Mono-and Tetra-nuclear copper complexes bearing bis(imino)phenoxide
 derived ligands: catalytic evaluation for benzene oxidation and ROP of
 epsilon-caprolactone
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA08696E
_journal_year                    2015
_chemical_formula_moiety
;
4(C80 H106 Cu4 N4 O11), 4(C2 N), 11(C2 H3 N)
;
_chemical_formula_sum            'C350 H457 Cu16 N31 O44'
_chemical_formula_weight         6819.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2014-12-21 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   14.2390(6)
_cell_length_b                   51.092(2)
_cell_length_c                   14.3358(5)
_cell_measurement_reflns_used    35374
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      1.6
_cell_volume                     9138.7(7)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1154
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48175
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.285
_diffrn_reflns_theta_min         1.594
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7208
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Empirical absorption within Sortav
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             3590
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1980
_refine_ls_number_reflns         27844
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2448
_reflns_Friedel_coverage         0.977
_reflns_friedel_fraction_full    0.990
_reflns_friedel_fraction_max     0.986
_reflns_number_gt                12557
_reflns_number_total             27844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra08696e2.cif
_cod_data_source_block           2-2-2
_cod_database_code               7220720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.745
_shelx_res_checksum              40870