Formation of a Hexacarbonyl Diiron Complex Having a Naphthalene-1,8-bis(phenylphosphido) Bridge and the Electrochemical Behavior of Its Derivatives
Teramoto, Yuichi; Kubo, Kazuyuki; Kume, Shoko; Mizuta, Tsutomu; Organometallics 32 (2013) 7014–; doi:10.1021/om4006142

data_4081829
_publ_section_title
;
 Formation of a Hexacarbonyl Diiron Complex Having a
 Naphthalene-1,8-bis(phenylphosphido) Bridge and the Electrochemical
 Behavior of Its Derivatives
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7014
_journal_paper_doi               10.1021/om4006142
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C30.5 H17 Cl Fe2 O8 P2'
_chemical_formula_weight         720.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.0940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.019(3)
_cell_length_b                   17.875(2)
_cell_length_c                   17.0427(19)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.33
_cell_volume                     6186.2(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18083
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.8914
_exptl_absorpt_correction_T_min  0.8433
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Sheldrick 1996 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7307
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+5.7927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                5889
_reflns_number_total             7307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4006142_si_002.cif
_cod_data_source_block           teramoto03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6186.3(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30.50 H17 Cl Fe2 O8 P2'
_cod_database_code               4081829