Reaction of metallophosphanide anions with MLnX (X = halide) species as a simple route to heterometallic transition metal complexes
Birte Ahrens; Jacqueline M. Cole; Jonathan P. Hickey; James N. Martin; Martin J. Mays; Paul R. Raithby; Simon J. Teat; Anthony D. Woods; Dalton Trans.  (2003) 1389–1395; doi:10.1039/b211243d

data_7012475
_publ_section_title
;
 Reaction of metallophosphanide anions with MLnX (X = halide) species
 as a simple route to heterometallic transition metal complexes
;
_journal_issue                   7
_journal_name_full               'Dalton Trans.'
_journal_page_first              1389
_journal_page_last               1395
_journal_paper_doi               10.1039/b211243d
_journal_year                    2003
_chemical_formula_sum            'C32 H22 Fe O12 Os3 P'
_chemical_formula_weight         1255.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.537(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9577(19)
_cell_length_b                   10.834(2)
_cell_length_c                   34.169(7)
_cell_measurement_reflns_used    14240
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.96
_cell_volume                     3305.6(12)
_computing_cell_refinement       'LSCELL (CLEGG, 1997)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'XP (Sheldrick, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice, \w-scans'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source
'Synchrotron Radiation Source, Daresbury Laboratories, UK'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.69230
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            22341
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.036
_exptl_absorpt_correction_T_max  0.7948
_exptl_absorpt_correction_T_min  0.5320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'from symmetry-related measurements, SORTAV (Blessing 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.689
_refine_diff_density_min         -3.395
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    'methyl rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8711
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+38.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                6792
_reflns_number_total             8711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211243d.txt
_cod_data_source_block           for_complex_9
_cod_original_cell_volume        3305.7(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012475