3,4-Dimethyl-2-phenyl-1-phosphaferrocene
Scheibitz, Mathias; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 63 (2007) m1118–m1119; doi:10.1107/S1600536807012214

data_2212757
_publ_section_title
;
 3,4-Dimethyl-2-phenyl-1-phosphaferrocene
;
_journal_coeditor_code           AT2240
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1118
_journal_page_last               m1119
_journal_paper_doi               10.1107/S1600536807012214
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Fe (C5 H5) (C12 H12 P)]'
_chemical_formula_moiety         'C17 H17 Fe P'
_chemical_formula_sum            'C17 H17 Fe P'
_chemical_formula_weight         308.13
_chemical_name_systematic
;
3,4-Dimethyl-2-phenyl-1-phosphaferrocene
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4305(4)
_cell_length_b                   8.2000(5)
_cell_length_c                   23.0148(9)
_cell_measurement_reflns_used    65535
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      2.6
_cell_volume                     1402.29(13)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42005
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         29.80
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.8820
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.567
_refine_ls_abs_structure_details 'Flack (1983), with 1689 Friedel pairs'
_refine_ls_abs_structure_Flack   0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0390P)^2^+0.2803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3898
_reflns_number_total             3998
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2240.cif
_cod_data_source_block           I
_cod_database_code               2212757
_cod_database_fobs_code          2212757