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_4314255
_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 Co3 N12 O6 P2 S2'
_chemical_formula_weight         1549.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.370(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.259(2)
_cell_length_b                   27.074(2)
_cell_length_c                   21.830(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.99
_cell_measurement_theta_min      5.28
_cell_volume                     6565.6(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14776
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.8111
_exptl_absorpt_correction_T_min  0.4327
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       large_plate
_exptl_crystal_F_000             3140
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.99
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00034(10)
_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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         14184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          2.302
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+3.5790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                8323
_reflns_number_total             14184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034434hsi20030714_033817_3.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        6565.2(16)
_cod_database_code               4314255