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_4302981
_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            'C91.5 H80 Cl6 Fe4 O4 P4'
_chemical_formula_weight         1803.54
_chemical_name_systematic
; 
 ? 
;
_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                69.9960(10)
_cell_angle_beta                 69.6210(10)
_cell_angle_gamma                62.0370(10)
_cell_formula_units_Z            2
_cell_length_a                   16.8980(4)
_cell_length_b                   17.2740(4)
_cell_length_c                   17.3800(5)
_cell_measurement_temperature    200(2)
_cell_volume                     4101.29(18)
_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 0.886
_diffrn_measured_fraction_theta_max 0.886
_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    0.0657
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17507
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.9364
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0042(3)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         17507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0594P)^2^+17.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                11007
_reflns_number_total             17507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9013224_si_002_1.cif
_cod_data_source_block           inami02
_cod_original_cell_volume        4101.30(18)
_cod_original_formula_sum        'C91.50 H80 Cl6 Fe4 O4 P4'
_cod_database_code               4302981