Isomerization Mechanisms of Stereolabile tris- and bis-Bidentate Octahedral Cobalt(II) Complexes: X-ray Structure and Variable Temperature and Pressure NMR Kinetic Investigations
Fabrice Riblet; Ghenadie Novitchi; Rosario Scopelliti; Lothar Helm; Aurelian Gulea; André E. Merbach; Inorganic Chemistry 49 (2010) 4194–4211; doi:10.1021/ic902494j

data_4315464
_publ_contact_author_address
;Ecole polytechnique f\'ed\'erale de Lausanne
Institut des sciences et ing\'enierie chimiques
EPFL SB ISIC LCIB
BCH 3108 (B\^at. BCH)
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       lothar.helm@epfl.ch
_publ_contact_author_fax         '+41 21 693 98 55'
_publ_contact_author_name        'Lothar Helm'
_publ_contact_author_phone       '+41 21 693 98 75'
_publ_section_title
;
 Isomerization Mechanisms of Stereolabile tris- and bis-Bidentate
 Octahedral Cobalt(II) Complexes: X-ray Structure and Variable Temperature
 and Pressure NMR Kinetic Investigations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4194
_journal_page_last               4211
_journal_paper_doi               10.1021/ic902494j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H16 Co F12 N2 O4'
_chemical_formula_sum            'C22 H16 Co F12 N2 O4'
_chemical_formula_weight         659.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6976(9)
_cell_length_b                   16.3685(15)
_cell_length_c                   15.9331(18)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.0182
_cell_measurement_theta_min      2.47825
_cell_volume                     2529.1(4)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction KM4/Sapphire CCD'
_diffrn_measurement_method       'phi and omega 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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7626
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                1069
_reflns_number_total             1235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902494j_si_001_3.cif
_cod_data_source_block           nov36a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315464