(2<i>S</i>,4<i>S</i>,<i>S</i>~Fc~)-2-[2-(Diphenylthiophosphinoyl)ferrocenyl]-4-methoxymethyl-1,3-dioxane
Jean-Claude Daran; Eric Manoury; Lucie Routaboul; Frédéric Rivals; Acta Crystallographica Section C 62 (2006) m378–m380; doi:10.1107/S0108270106025662

data_2015524
_publ_section_title
(2<i>S</i>,4<i>S</i>,<i>S</i>~Fc~)-2-[2-(Diphenylthiophosphinoyl)ferrocenyl]-4-methoxymethyl-1,3-dioxane
_journal_coeditor_code           SQ3026
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m378
_journal_page_last               m380
_journal_paper_doi               10.1107/S0108270106025662
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe (C5 H5) (C23 H24 O3 P S)]'
_chemical_formula_moiety         'C28 H29 Fe O3 P S'
_chemical_formula_sum            'C28 H29 Fe O3 P S'
_chemical_formula_weight         532.39
_chemical_name_systematic
(2S,4S,S~Fc~)-2-[(Diphenylthiophosphino)ferrocenyl]-4-methoxymethyl-1,3-dioxane
_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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.4886(12)
_cell_length_b                   15.2217(17)
_cell_length_c                   17.071(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      1.79
_cell_volume                     2465.6(5)
_computing_cell_refinement       'IPDS Software'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'XRED (Stoe & Cie, 1996)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19961
_diffrn_reflns_theta_full        24.33
_diffrn_reflns_theta_max         24.33
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  8
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.312
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   -0.016(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                3266
_reflns_number_total             3962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3026.cif
_cod_data_source_block           I
_cod_original_cell_volume        2465.7(5)
_cod_database_code               2015524
_cod_database_fobs_code          2015524