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_4329140
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C62 H62 Co2 N4 O6 P3, Cl O4'
_chemical_formula_sum            'C62 H62 Cl Co2 N4 O10 P3'
_chemical_formula_weight         1269.38
_chemical_name_systematic
;
1 at 100
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22T14:30:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.5260(10)
_cell_length_b                   13.5260(10)
_cell_length_c                   57.341(4)
_cell_measurement_reflns_used    3290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.338
_cell_measurement_theta_min      2.2454
_cell_measurement_wavelength     0.71073
_cell_volume                     9085.2(11)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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      -0.434124E-1
_diffrn_orient_matrix_UB_12      -0.819597E-1
_diffrn_orient_matrix_UB_13      0.484888E-2
_diffrn_orient_matrix_UB_21      -0.761422E-2
_diffrn_orient_matrix_UB_22      -0.238657E-1
_diffrn_orient_matrix_UB_23      -0.167143E-1
_diffrn_orient_matrix_UB_31      0.731168E-1
_diffrn_orient_matrix_UB_32      -0.130543E-2
_diffrn_orient_matrix_UB_33      0.113838E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            14927
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.07
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             3948
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.7
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+44.5616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                3489
_reflns_number_total             5028
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3004799_si_002_3.cif
_cod_data_source_block           11mz390_0m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4329140