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_4329138
_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         'C52.17 H52.14 Co2 N3 O9 P3, 2.33(C H Cl3)'
_chemical_formula_sum            'C54.5 H54.47 Cl7 Co2 N3 O9 P3'
_chemical_formula_weight         1354.02
_chemical_name_systematic
;
3
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22T14:57:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.314(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.958(2)
_cell_length_b                   20.615(3)
_cell_length_c                   20.993(3)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5302
_cell_measurement_theta_min      2.214
_cell_measurement_wavelength     0.71073
_cell_volume                     6324.5(15)
_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      293(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.429548E-1
_diffrn_orient_matrix_UB_12      -0.103725E-1
_diffrn_orient_matrix_UB_13      -0.292283E-1
_diffrn_orient_matrix_UB_21      -0.292892E-1
_diffrn_orient_matrix_UB_22      0.344199E-1
_diffrn_orient_matrix_UB_23      -0.03121
_diffrn_orient_matrix_UB_31      0.445334E-1
_diffrn_orient_matrix_UB_32      0.326425E-1
_diffrn_orient_matrix_UB_33      0.236218E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63580
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             2769
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         15684
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0889P)^2^+8.9127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.153
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                11694
_reflns_number_total             15684
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3004799_si_002_1.cif
_cod_data_source_block           11mz382_0m
_cod_original_cell_volume        6324.3(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C54.50 H54.47 Cl7 Co2 N3 O9 P3'
_cod_database_code               4329138