Three new enantiomerically pure ferrocenylphosphole compounds
José Guadalupe Lopez Cortes; Sandrine Vincendeau; Jean-Claude Daran; Eric Manoury; Maryse Gouygou; Acta Crystallographica Section C 62 (2006) m188–m191; doi:10.1107/S0108270106010833

data_2015328
_publ_section_title
;
 Three new enantiomerically pure ferrocenylphosphole compounds
;
_journal_coeditor_code           SK3012
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m188
_journal_page_last               m191
_journal_paper_doi               10.1107/S0108270106010833
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe (C5 H5) (C23 H22 O3 P S)]'
_chemical_formula_moiety         'C28 H27 Fe O3 P S'
_chemical_formula_sum            'C28 H27 Fe O3 P S'
_chemical_formula_weight         530.38
_chemical_name_systematic
;
(2S,4S,SFc)-4-(methoxymethyl)-2-[(2-dibenzo-1-thio-1H-1\l^5^-
phosphol-1-yl)ferrocenyl]-1,3-dioxane
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 91.067(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4885(7)
_cell_length_b                   9.5175(8)
_cell_length_c                   16.8193(13)
_cell_measurement_reflns_used    3139
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.63
_cell_measurement_theta_min      3.63
_cell_volume                     1198.53(18)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_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_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford XCALIBUR'
_diffrn_measurement_method       '\w and \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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10617
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.330
_refine_ls_abs_structure_details 'Flack (1983), with 1249 Friedel pairs'
_refine_ls_abs_structure_Flack   0.000(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4383
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0401P)^2^+0.0522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                4045
_reflns_number_total             4383
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3012.cif
_cod_data_source_block           III
_cod_database_code               2015328
_cod_database_fobs_code          2015328