Synthesis of a Hetero-bimetallic Complex with an Inorganic Cyclic Framework Using a Bis(iminophosphorane)iron Complex as a Chelating Ligand
Kubo, Kazuyuki; Akimoto, Takashi; Mizuta, Tsutomu; Miyoshi, Katsuhiko; Chemistry Letters 37 (2008) 166–; doi:10.1246/cl.2008.166

data_8000181
_publ_section_title
;
 Synthesis of a Hetero-bimetallic Complex with an Inorganic Cyclic
 Framework Using a Bis(iminophosphorane)iron Complex as a Chelating Ligand
;
_journal_issue                   2
_journal_name_full               'Chemistry Letters'
_journal_page_first              166
_journal_paper_doi               10.1246/cl.2008.166
_journal_volume                  37
_journal_year                    2008
_chemical_formula_sum            'C35 H49 Fe N2 O5 P2 Rh'
_chemical_formula_weight         798.46
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6590(3)
_cell_length_b                   15.6820(3)
_cell_length_c                   19.6260(6)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_volume                     3588.35(16)
_computing_cell_refinement       HKL
_computing_data_collection       HKL
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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    0.0401
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7799
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0240P)^2^+14.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                7005
_reflns_number_total             7799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            37-166sup1.cif
_cod_data_source_block           4
_cod_database_code               8000181