Dicarbonyldichloridobis(trimethylphosphane)iron(II)–carbonyldichloridotris(trimethylphosphane)iron(II)–tetrahydrofuran (1/1/2)
Rath, Nigam P.; Stouffer, Meghan; Janssen, Matthew K.; Bleeke, John R.; Acta Crystallographica Section E 67 (2011) m462–; doi:10.1107/S1600536811009305

data_2229802
_publ_section_title
;
 Dicarbonyldichloridobis(trimethylphosphane)iron(II)--carbonyldichloridotris(trimethylphosphane)iron(II)--tetrahydrofuran
 (1/1/2)
;
_journal_coeditor_code           PV2394
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m462
_journal_paper_doi               10.1107/S1600536811009305
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Fe Cl2 (C3 H9 P)3 (C O)], [Fe Cl2 (C3 H9 P)2 (C O)2], 2C4 H8 O'
_chemical_formula_moiety
'C10 H27 Cl2 Fe O P3, C8 H18 Cl2 Fe O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C26 H61 Cl4 Fe2 O5 P5'
_chemical_formula_weight         862.10
_chemical_name_systematic
;
Dicarbonyldichloridobis(trimethylphosphane)iron(II)--
carbonyldichloridotris(trimethylphosphane)iron(II)--tetrahydrofuran (1/1/2)
;
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   10.8391(9)
_cell_length_b                   16.9670(12)
_cell_length_c                   22.2871(18)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.62
_cell_volume                     4098.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and Mercury (Macrae, <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0899
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            144514
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.8950
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.702
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0323P)^2^+5.0170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                3939
_reflns_number_total             4904
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2394.cif
_cod_data_source_block           I
_cod_database_code               2229802
_cod_database_fobs_code          2229802