Structural Study of Mixed Crystals of [Zn1-xRux(bpy)3][NaCr(ox)3] Probed by High-Resolution Absorption Spectroscopy and High-Pressure Experiments
Mia Milos; Tiphaine Penhouet; Prodipta Pal; Andreas Hauser; Inorganic Chemistry 49 (2010) 3402–3408; doi:10.1021/ic902514w

data_4315297
_publ_section_title
;
 Structural Study of Mixed Crystals of [Zn1-xRux(bpy)3][NaCr(ox)3] Probed
 by High-Resolution Absorption Spectroscopy and High-Pressure Experiments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3402
_journal_page_last               3408
_journal_paper_doi               10.1021/ic902514w
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 Cr Na O12, C30 H24 N6 Ru'
_chemical_formula_sum            'C36 H24 Cr N6 Na O12 Ru'
_chemical_formula_weight         908.68
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5098(6)
_cell_length_b                   15.5098(6)
_cell_length_c                   15.5098(6)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.25
_cell_volume                     3730.9(2)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3349
_diffrn_reflns_theta_full        28.093
_diffrn_reflns_theta_max         29.152
_diffrn_reflns_theta_min         2.274
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
 Gaussian Integration (Busing and Levy, 1957) 
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1828.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack (1983), 1498 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8736
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.0003425
_refine_ls_shift/su_mean         3.2972901
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 21.4 24.8 14.8 4.44 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0662
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              1
_reflns_number_gt                2302
_reflns_number_total             3349
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.79
_oxford_diffrn_Wilson_scale      14.72
_oxford_refine_ls_r_factor_ref   0.0492
_oxford_refine_ls_scale          0.2879(2)
_oxford_reflns_number_all        2442
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic902514w_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21 3 '
_cod_original_formula_sum        'C36 H24 Cr1 N6 Na1 O12 Ru1'
_cod_database_code               4315297