Synthesis of Binuclear Complexes Bound in an Enlarged Tetraphosphamacrocycle: Two Diphosphine Metal Units Linked in Front-to-Front Style
Tsutomu Mizuta; Yuta Inami; Kazuyuki Kubo; Katsuhiko Miyoshi; Inorganic Chemistry 48 (2009) 7534–7536; doi:10.1021/ic9013224

data_4302982
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, 
Hiroshima University, 
1-3-1 Kagamiyama, Higashi-Hiroshima 739-8526, JAPAN
;
_publ_contact_author_email       mizuta@sci.hiroshima-u.ac.jp
_publ_contact_author_fax         +81-824-24-0729
_publ_contact_author_name        'Prof Tsutomu Mizuta'
_publ_contact_author_phone       +81-824-24-7420
_publ_section_title
;
Synthesis of Binuclear Complexes Bound in an Enlarged
Tetraphosphamacrocycle: Two Diphosphine Metal Units Linked in
Front-to-Front Style
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7534
_journal_page_last               7536
_journal_paper_doi               10.1021/ic9013224
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C82 H78 Ag2 B2 F8 Fe4 N6 O4 P4'
_chemical_formula_weight         1948.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   32.2330(4)
_cell_length_b                   32.233
_cell_length_c                   47.9690(7)
_cell_measurement_temperature    200(2)
_cell_volume                     43161.1(8)
_computing_cell_refinement       'HKL (Otwinowski, 1997)'
_computing_data_collection       'HKL (Otwinowski, 1997)'
_computing_data_reduction        'HKL (Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Mac Science DIP2030 Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            16854
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.8732
_exptl_absorpt_correction_T_min  0.8281
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17712
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.000066(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   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         16854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0831P)^2^+383.7046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1880
_reflns_number_gt                13776
_reflns_number_total             16854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9013224_si_002_2.cif
_cod_data_source_block           inami05
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4302982