Copper/TEMPO-Catalyzed Aerobic Alcohol Oxidation: Mechanistic Assessment of Different Catalyst Systems
Hoover, Jessica M.; Ryland, Bradford L.; Stahl, Shannon S.; ACS Catalysis 3 (2013) 2599–; doi:10.1021/cs400689a

data_4508379
_publ_section_title
;
 Copper/TEMPO-Catalyzed Aerobic Alcohol Oxidation: Mechanistic Assessment
 of Different Catalyst Systems
;
_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              2599
_journal_paper_doi               10.1021/cs400689a
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C44 H36 Cu4 F12 N8 O16 S4'
_chemical_formula_sum            'C44 H36 Cu4 F12 N8 O16 S4'
_chemical_formula_weight         1543.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.624(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.452(4)
_cell_length_b                   13.8983(17)
_cell_length_c                   15.856(3)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.3336
_cell_measurement_theta_min      3.5894
_cell_volume                     5427.2(15)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.70\% \w and 0.7\% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69787
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.09
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    4.272
_exptl_absorpt_correction_T_max  0.7102
_exptl_absorpt_correction_T_min  0.5591
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         10448
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+8.5674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                8082
_reflns_number_total             10448
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cs400689a_si_001.cif
_cod_data_source_block           stahl119
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1  '
_cod_database_code               4508379