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_4314257
_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            'C52 H52 Cl12 N12 O6 P2 S2 Zn3'
_chemical_formula_weight         1688.63
_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_creation_method           SHELXL-97
_cell_angle_alpha                72.971(8)
_cell_angle_beta                 82.029(12)
_cell_angle_gamma                74.454(8)
_cell_formula_units_Z            2
_cell_length_a                   11.166(6)
_cell_length_b                   15.138(8)
_cell_length_c                   21.243(10)
_cell_measurement_temperature    150(2)
_cell_volume                     3301(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20802
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.987
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         14443
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1197P)^2^+17.0103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                11985
_reflns_number_total             14443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034434hsi20030714_033817_5.cif
_cod_data_source_block           Compound_6
_cod_database_code               4314257