One- and Two-Electron Reduced 1,2-Diketone Ligands in [CrIII(L.)3] (S= 0) and Na2(Et2O)2[VIV(LRed)3] (S=1/2)
Geoffrey H. Spikes; Stephen Sproules; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 47 (2008) 10935–10944; doi:10.1021/ic801122m

data_4306280
_publ_section_title
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One- and Two-Electron Reduced 1,2-Diketone Ligands in [CrIII(L.)3] (S= 0)
and Na2(Et2O)2[VIV(LRed)3] (S=1/2)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10935
_journal_page_last               10944
_journal_paper_doi               10.1021/ic801122m
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C78 H102 Cr O6'
_chemical_formula_weight         1187.60
_space_group_IT_number           15
_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                 92.448(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8701(3)
_cell_length_b                   27.5230(7)
_cell_length_c                   23.5899(6)
_cell_measurement_temperature    100(2)
_cell_volume                     7051.1(3)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method
'2415 images at 0.5 deg. stepwise rotation in omega and phi, 25 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 45 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            86908
_diffrn_reflns_theta_full        33.27
_diffrn_reflns_theta_max         33.27
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            'redish brown'
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         13550
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+5.1058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                11070
_reflns_number_total             13550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801122m_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4306280