Electronic and Molecular Structure of High-Spin d4 Complexes: Experimental and Theoretical Study of the [Cr(D2O)6]2+ Cation in Tutton's Salts
Christopher Dobe; Christopher Noble; Graham Carver; Philip L. W. Tregenna-Piggott; Garry J. McIntyre; Anne-Laure Barra; Antonia Neels; Stefan Janssen; Fanni Juranyi; Journal of the American Chemical Society 126 (2004) 16639–16652; doi:10.1021/ja046095c

data_4113286
_publ_section_title
;
 Electronic and Molecular Structure of High-Spin d4 Complexes:
 Experimental and Theoretical Study of the [Cr(D2O)6]2+ Cation in Tutton's
 Salts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16639
_journal_page_last               16652
_journal_paper_doi               10.1021/ja046095c
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'Cr Cs2 H12 O14 S2'
_chemical_formula_weight         618.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.135(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.3181(11)
_cell_length_b                   12.8039(15)
_cell_length_c                   9.4930(16)
_cell_measurement_reflns_used    22677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      1.14
_cell_volume                     737.7(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12995
_diffrn_reflns_theta_full        29.54
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    5.983
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.169
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'PLATON99 (Spek, 1990)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0000P)^2^+4.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                1790
_reflns_number_total             2032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046095csi20040701_120017.cif
_cod_data_source_block           cscrh-lt
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4113286