Assembly of Triangular Trimetallic Complexes by Triamidophosphine Ligands: Spin-Frustrated Mn2+ Plaquettes and Diamagnetic Mg2+ Analogues with a Combined Through-Space, Through-Bond Pathway for 31P-31P Spin-Spin Coupling
Jillian A. Hatnean; Ritu Raturi; Julie Lefebvre; Daniel B. Leznoff; Gavin Lawes; Samuel A. Johnson; Journal of the American Chemical Society 128 (2006) 14992–14999; doi:10.1021/ja065597i

data_4111106
_publ_section_title
;
 Assembly of Triangular Trimetallic Complexes by Triamidophosphine
 Ligands: Spin-Frustrated Mn2+ Plaquettes and Diamagnetic Mg2+ Analogues
 with a Combined Through-Space, Through-Bond Pathway for 31P-31P Spin-Spin
 Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14992
_journal_page_last               14999
_journal_paper_doi               10.1021/ja065597i
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C60 H78 Mn3 N6 O4.5 P2'
_chemical_formula_weight         1182.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2006-06-23T16:20:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.3530(10)
_cell_angle_beta                 81.8870(10)
_cell_angle_gamma                84.5170(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8336(10)
_cell_length_b                   13.3050(13)
_cell_length_c                   22.388(2)
_cell_measurement_reflns_used    8615
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.34
_cell_volume                     2882.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32597
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       cut
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.524
_refine_diff_density_min         -0.78
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         12815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0954P)^2^+1.7453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                10516
_reflns_number_total             12815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065597isi20060914_103126.cif
_cod_data_source_block           jhmnphs
_cod_original_formula_sum        'C60 H78 Mn3 N6 O4.50 P2'
_cod_database_code               4111106