Structural Insights into Ligand Dynamics: Correlated Oxygen and Picket Motion in Oxycobalt Picket Fence Porphyrins
Jianfeng Li; Bruce C. Noll; Allen G. Oliver; W. Robert Scheidt; Journal of the American Chemical Society 134 (2012) 10595–10606; doi:10.1021/ja303475a

data_4118142
_publ_section_title
;
 Structural Insights into Ligand Dynamics: Correlated Oxygen and Picket
 Motion in Oxycobalt Picket Fence Porphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10595
_journal_page_last               10606
_journal_paper_doi               10.1021/ja303475a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C68 H70 Co N10 O6, 1.8(C2 H6 O)'
_chemical_formula_sum            'C71.6 H80.8 Co N10 O7.8'
_chemical_formula_weight         1265.19
_chemical_name_common            '[Co(TpivPP)(2-MeIm)(O2)]1.8EtOH'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.0650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7514(3)
_cell_length_b                   19.5309(3)
_cell_length_c                   17.8719(3)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7457
_cell_measurement_theta_min      2.7491
_cell_volume                     6544.13(18)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2007; Sheldrick, 2008)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'XCIF (Sheldrick, 2008)/enCIFer (CCDC, 2005)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Brucker d8 ApexII CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68291
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9497
_exptl_absorpt_correction_T_min  0.8889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             2679
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10425
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+9.1218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                8732
_reflns_number_total             10425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303475a_si_008.cif
_cod_data_source_block           jfli-d8-002-0m
_cod_original_formula_sum        'C71.60 H80.80 Co N10 O7.80'
_cod_database_code               4118142