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_4111103
_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_moiety         'C54 H66 Mg3 N6 O3 P2, 2.5(C6 H6)'
_chemical_formula_sum            'C69 H81 Mg3 N6 O3 P2'
_chemical_formula_weight         1177.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2006-06-23T16:10:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.937(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.882(4)
_cell_length_b                   9.5933(13)
_cell_length_c                   25.776(3)
_cell_measurement_reflns_used    6577
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.12
_cell_measurement_theta_min      2.27
_cell_volume                     6287.5(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58371
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         0.8
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       plate
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         11073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0468P)^2^+8.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.14
_reflns_number_gt                7729
_reflns_number_total             11073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065597isi20060914_094949.cif
_cod_data_source_block           rr2981m
_cod_original_cell_volume        6287.4(14)
_cod_database_code               4111103