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_4314254
_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            'C51 H51 Cl9 Mn3 N12 O6 P2 S2'
_chemical_formula_weight         1537.97
_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                83.729(9)
_cell_angle_beta                 72.136(9)
_cell_angle_gamma                62.092(7)
_cell_formula_units_Z            1
_cell_length_a                   11.048(6)
_cell_length_b                   11.100(6)
_cell_length_c                   15.767(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1624.9(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker AXS Smart Apex'
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6359
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             779
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.360
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4146
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.1138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1778P)^2^+28.3869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3034
_refine_ls_wR_factor_ref         0.3166
_reflns_number_gt                3093
_reflns_number_total             4146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034434hsi20030714_033817_2.cif
_cod_data_source_block           Compound_3
_cod_original_cell_volume        1624.9(14)
_cod_database_code               4314254