A Phosphorus Supported Multisite Coordinating Tris Hydrazone P(S)[N(Me)NCHC6H4-o-OH]3 as an Efficient Ligand for the Assembly of Trinuclear Metal Complexes: Synthesis, Structure, and Magnetism
Vadapalli Chandrasekhar; Ramachandran Azhakar; Gurusamy Thanagavelu Senthil Andavan; Venkatasubbaiah Krishnan; Stefano Zacchini; Jamie F. Bickley; Alexander Steiner; Raymond J. Butcher; Paul Kögerler; Inorganic Chemistry 42 (2003) 5989–5998; doi:10.1021/ic034434h

data_4314256
_publ_section_title
;
 A Phosphorus Supported Multisite Coordinating Tris Hydrazone
 P(S)[N(Me)NCHC6H4-o-OH]3 as an Efficient Ligand for the Assembly of
 Trinuclear Metal Complexes: Synthesis, Structure, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5989
_journal_page_last               5998
_journal_paper_doi               10.1021/ic034434h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C50 H50 Cl6 N12 Ni3 O6 P2 S2'
_chemical_formula_weight         1429.91
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.175(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.866(3)
_cell_length_b                   11.7893(13)
_cell_length_c                   28.012(4)
_cell_measurement_temperature    213(2)
_cell_volume                     5952.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18655
_diffrn_reflns_theta_full        24.24
_diffrn_reflns_theta_max         24.24
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_meas      0.3
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          orange
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                3589
_reflns_number_total             4730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034434hsi20030714_033817_4.cif
_cod_data_source_block           Compound_5
_cod_database_code               4314256