Chiral tetranuclear and dinuclear copper(ii) complexes for TEMPO-mediated aerobic oxidation of alcohols: are four metal centres better than two?
Zhang, Guoqi; Proni, Gloria; Zhao, Sherry; Constable, Edwin C.; Housecroft, Catherine E.; Neuburger, Markus; Zampese, Jennifer A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12313–12320; doi:10.1039/c4dt01224k

data_7031490
_publ_section_title
;
 Chiral tetranuclear and dinuclear copper(ii) complexes for TEMPO-mediated
 aerobic oxidation of alcohols: are four metal centres better than two?
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12313
_journal_page_last               12320
_journal_paper_doi               10.1039/c4dt01224k
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C92 H116 Cu4 N4 O8, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C93.5 H119 Cl3 Cu4 N4 O8'
_chemical_formula_weight         1787.43
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.095(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.255(2)
_cell_length_b                   17.369(2)
_cell_length_c                   12.8760(13)
_cell_measurement_reflns_used    11297
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      47.35
_cell_measurement_theta_min      4.14
_cell_volume                     4611.7(9)
_computing_cell_refinement       'Stoe IPDS'
_computing_data_collection       'Stoe IPDS'
_computing_data_reduction        'Stoe IPDS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            91084
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.495
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing 1951)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.030(13)
_refine_ls_extinction_coef       0.0074(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11623
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0532P)^2^+5.1514P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11525
_reflns_number_total             11623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01224k1.cif
_cod_data_source_block           (R)-1
_cod_depositor_comments
'Adding full bibliography for 7031490--7031491.cif.'
_cod_original_formula_sum        'C93.50 H119 Cl3 Cu4 N4 O8'
_cod_database_code               7031490
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.817
_shelxl_version_number           2013-2
_shelx_res_checksum              92580
_shelx_hkl_checksum              22552