Synthesis and Characterization of Benzo[b]phosphaferrocene Derivatives
Ogasawara, Masamichi; Arae, Sachie; Watanabe, Susumu; Subbarayan, Velusamy; Sato, Hiroyasu; Takahashi, Tamotsu; Organometallics 32 (2013) 4997–; doi:10.1021/om400496b

data_4081290
_publ_section_title
;
 Synthesis and Characterization of Benzo[b]phosphaferrocene Derivatives
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4997
_journal_paper_doi               10.1021/om400496b
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C17 H21 Fe P Si'
_chemical_formula_sum            'C17 H21 Fe P Si'
_chemical_formula_weight         340.26
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.274(2)
_cell_length_b                   11.667(3)
_cell_length_c                   16.840(5)
_cell_measurement_reflns_used    5416
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     1625.6(7)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r15'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r15'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6554
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712.00
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1518 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.575(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                3156
_reflns_number_total             3644
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om400496b_si_002.cif
_cod_data_source_block           SX114
_cod_database_code               4081290