Anionic Phospho-Fries Rearrangement at Ferrocene: One-Pot Approach to P,O-Substituted Ferrocenes
Korb, Marcus; Schaarschmidt, Dieter; Lang, Heinrich; Organometallics 33 (2014) 2099–; doi:10.1021/om5002827

data_4082957
_publ_section_title
;
 Anionic Phospho-Fries Rearrangement at Ferrocene: One-Pot Approach to
 P,O-Substituted Ferrocenes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2099
_journal_paper_doi               10.1021/om5002827
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C16 H19 P S'
_chemical_formula_sum            'C16 H19 P S'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.089(6)
_cell_angle_beta                 88.870(6)
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_cell_length_a                   9.1715(7)
_cell_length_b                   11.9513(8)
_cell_length_c                   13.8640(10)
_cell_measurement_reflns_used    4482
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      28.8710
_cell_measurement_theta_min      3.5360
_cell_volume                     1476.34(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110.00(10)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '\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  0.0700
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9738
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.776
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     327
_refine_ls_number_reflns         5158
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1690P)^2^+0.2517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2353
_refine_ls_wR_factor_ref         0.2484
_reflns_number_gt                4291
_reflns_number_total             5158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5002827_si_001.cif
_cod_data_source_block           mk-226
_cod_depositor_comments
'Adding full bibliography for 4082955--4082957.cif.'
_cod_original_cell_volume        1476.34(18)
_cod_database_code               4082957