Solid-State NMR of a Paramagnetic DIAD-FeII Catalyst: Sensitivity, Resolution Enhancement, and Structure-Based Assignments
Gwendal Kervern; Guido Pintacuda; Yong Zhang; Eric Oldfield; Charbel Roukoss; Emile Kuntz; Eberhardt Herdtweck; Jean-Marie Basset; Sylvian Cadars; Anne Lesage; Christophe Copéret; Lyndon Emsley; Journal of the American Chemical Society 128 (2006) 13545–13552; doi:10.1021/ja063510n

data_4110966
_publ_contact_author
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       Dr. Eberhardt Herdtweck,
       Department Chemie,
       Lehrstuhl f\"ur Anorganische Chemie,
       Technische Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
 Solid-State NMR of a Paramagnetic DIAD-FeII Catalyst: Sensitivity,
 Resolution Enhancement, and Structure-Based Assignments
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13545
_journal_page_last               13552
_journal_paper_doi               10.1021/ja063510n
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C28 H40 Cl2 Fe N2'
_chemical_formula_sum            'C28 H40 Cl2 Fe N2'
_chemical_formula_weight         531.37
_chemical_name_systematic        ?
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12-May-05
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
   12-May-05 Updated by the Author E.H.
             Text writing by E.H.
             Checkcif    OK
   12-May-05 Updated by the Author E.H.
   12-Apr-06 Updated by the Author E.H.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6185(2)
_cell_length_b                   21.3367(3)
_cell_length_c                   10.4310(1)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.91
_cell_volume                     2808.41(7)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            65010
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          1.14
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0237P)^2^+2.1064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                2504
_reflns_number_total             2646
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja063510nsi20060606_075718.cif
_cod_data_source_block           BLAB-4455-173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4110966