Syntheses and Structures of Three Complexes of Formulas [L3Co(μ2-O2P(Bn)2)3CoL'][L"], Featuring Octahedral and Tetrahedral Cobalt(II) Geometries; Variable-Temperature Magnetic Susceptibility Measurement and Analysis on [(py)3Co(μ2-O2PBn2)3Co(py)][ClO4]
John S. Maass; Matthias Zeller; Tanya M. Breault; Bart M. Bartlett; Hiroshi Sakiyama; Rudy L. Luck; Inorganic Chemistry 51 (2012) 4903–4905; doi:10.1021/ic3004799

data_4329141
_publ_contact_author_address
;
Department of Chemistry
Michigan Technological University
1400 Townsend Drive
Houghton, MI USA 49931
;
_publ_contact_author_email       rluck@mtu.edu
_publ_contact_author_fax         '(906)487 2061'
_publ_contact_author_name        'Luck, Rudy L.'
_publ_contact_author_phone       '(906)487 2309'
_publ_section_title
;
 Syntheses and Structures of Three Complexes of Formulas
 [L3Co(\m2-O2P(Bn)2)3CoL'][L"], Featuring Octahedral and Tetrahedral
 Cobalt(II) Geometries; Variable-Temperature Magnetic Susceptibility
 Measurement and Analysis on [(py)3Co(\m2-O2PBn2)3Co(py)][ClO4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4905
_journal_paper_doi               10.1021/ic3004799
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C57 H57 Cl Co2 N3 O6 P3'
_chemical_formula_sum            'C57 H57 Cl Co2 N3 O6 P3'
_chemical_formula_weight         1126.28
_chemical_name_systematic
;
2
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      197
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-23T16:38:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.760(2)
_cell_length_b                   22.760(2)
_cell_length_c                   22.760(2)
_cell_measurement_reflns_used    3817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.162
_cell_measurement_theta_min      2.5311
_cell_measurement_wavelength     0.71073
_cell_volume                     11790.1(18)
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.824752E-2
_diffrn_orient_matrix_UB_12      -0.430312E-1
_diffrn_orient_matrix_UB_13      -0.327126E-2
_diffrn_orient_matrix_UB_21      0.182425E-1
_diffrn_orient_matrix_UB_22      0.64946E-2
_diffrn_orient_matrix_UB_23      -0.394391E-1
_diffrn_orient_matrix_UB_31      0.391101E-1
_diffrn_orient_matrix_UB_32      0.604507E-2
_diffrn_orient_matrix_UB_33      0.190858E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       -1
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11048
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             4840
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
The unit cell contains 4 methylene chloride molecules which have been 
treated as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4823
_refine_ls_number_restraints     508
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+19.0960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.211
_refine_ls_wR_factor_ref         0.2441
_reflns_number_gt                2785
_reflns_number_total             4823
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3004799_si_002_4.cif
_cod_data_source_block           12mz023_0m
_cod_database_code               4329141