Metal Ion Scrambling in Hexanuclear M6(Et2NCO2)12 Complexes (M = Co, Mg). Synthesis, Solid State Structure, and Solution Dynamics of Heteronuclear ConMg6-n(Et2NCO2)12 Complexes
M. Tyler Caudle; Jason B. Benedict; Charles K. Mobley; Nicholas A. Straessler; Thomas L. Groy; Inorganic Chemistry 41 (2002) 3183–3190; doi:10.1021/ic025604d

data_4318125
_publ_section_title
;
 Metal Ion Scrambling in Hexanuclear M6(Et2NCO2)12 Complexes (M = Co, Mg).
 Synthesis, Solid State Structure, and Solution Dynamics of Heteronuclear
 ConMg6-n(Et2NCO2)12 Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3183
_journal_page_last               3190
_journal_paper_doi               10.1021/ic025604d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C60 H120 Co1.58 Mg4.42 N12 O24'
_chemical_formula_weight         1594.33
_chemical_name_systematic
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 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                   20.8064(10)
_cell_length_b                   25.1198(12)
_cell_length_c                   16.4196(8)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.48
_cell_volume                     8581.7(7)
_computing_cell_refinement       'SAINT V6.02A'
_computing_data_collection       'SMART V5.618'
_computing_data_reduction        'SAINT V6.02A'
_computing_molecular_graphics    'Bruker SHELXTL Ver. 5.1 (1997)'
_computing_publication_material  'Bruker SHELXTL Ver. 5.1 (1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\w scan'
_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  0.1219
_diffrn_reflns_av_sigmaI/netI    0.1111
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41109
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.5894
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular Parallelepiped'
_exptl_crystal_F_000             3407
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.689
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4931
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.695
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                1549
_reflns_number_total             4931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025604d_s2_1.cif
_cod_data_source_block           Co1.6Mg4.4
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_sg_symbol_H-M      'C c c a'
_cod_database_code               4318125