CO and O2 Binding to Pseudo-tetradentate Ligand-Copper(I) Complexes with a Variable N-Donor Moiety: Kinetic/Thermodynamic Investigation Reveals Ligand-Induced Changes in Reaction Mechanism
Heather R. Lucas; Gerald J. Meyer; Kenneth D. Karlin; Journal of the American Chemical Society 132 (2010) 12927–12940; doi:10.1021/ja104107q

data_4103051
_publ_section_title
;
 CO and O2 Binding to Pseudo-tetradentate Ligand-Copper(I) Complexes with
 a Variable N-Donor Moiety: Kinetic/Thermodynamic Investigation Reveals
 Ligand-Induced Changes in Reaction Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12927
_journal_page_last               12940
_journal_paper_doi               10.1021/ja104107q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C22 H20 Cu N4, C24 B F20'
_chemical_formula_sum            'C46 H20 B Cu F20 N4'
_chemical_formula_weight         1083.01
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Jan 16 14:34:05 2008'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.1276(2)
_cell_length_b                   20.3135(2)
_cell_length_c                   20.7405(2)
_cell_measurement_reflns_used    45558
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.2623
_cell_measurement_theta_min      3.9204
_cell_volume                     8480.00(14)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_publication_material  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega phi scans'
_diffrn_orient_matrix_UB_11      0.0329265492
_diffrn_orient_matrix_UB_12      -0.0062413677
_diffrn_orient_matrix_UB_13      0.0106590240
_diffrn_orient_matrix_UB_21      -0.0025186896
_diffrn_orient_matrix_UB_22      0.0265263934
_diffrn_orient_matrix_UB_23      0.0221507948
_diffrn_orient_matrix_UB_31      -0.0124250283
_diffrn_orient_matrix_UB_32      -0.0218741389
_diffrn_orient_matrix_UB_33      0.0237899889
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97989
_diffrn_reflns_resolution_max    0.75
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.93
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_voltage           50
_diffrn_standards_interval_count 2
_diffrn_standards_interval_time  50
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.7490
_exptl_crystal_size_mid          0.3925
_exptl_crystal_size_min          0.1980
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+12.6527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                7762
_reflns_number_total             10479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104107q_si_002.cif
_cod_data_source_block           BPQA
_cod_database_code               4103051
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_cell_measurement_resolution_max 0.71
_jhu_your_name_here              'Dr. Amy A Sarjeant'
_jhu_your_lab_here               'NCB 240'
_jhu_your_phone_number_here      x6-8569
_jhu_your_email_here             xray@jhu.edu
_jhu_institutional_source        'Karlin Lab'
_jhu_submitting_scientist        'Heather Lucas'
_jhu_scientist_phone             x6-6161
_jhu_scientist_email             hlucas4@jhu.edu
_jhu_identifying_number          x0418b
_jhu_xray_labbook                II-105
_jhu_crystalization_labbook
;
;
_jhu_crystalization_solvent
;
;
_jhu_crystalization_method
;
;
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              1