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_4315466
_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         'C28 H16 Co F12 N2 O4 S2, C7 H8'
_chemical_formula_sum            'C35 H24 Co F12 N2 O4 S2'
_chemical_formula_weight         887.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.473(14)
_cell_angle_beta                 101.131(15)
_cell_angle_gamma                110.333(19)
_cell_formula_units_Z            1
_cell_length_a                   9.337(2)
_cell_length_b                   9.6786(12)
_cell_length_c                   11.5297(17)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.204
_cell_measurement_theta_min      3.898
_cell_volume                     940.1(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19364
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10, G.M.Sheldrick, 2003'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             447
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0439P)^2^+2.2339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                3360
_reflns_number_total             4264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902494j_si_001_5.cif
_cod_data_source_block           nov35
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_cell_volume        940.2(3)
_cod_database_code               4315466