Direct Acetoacetylation of Ferrocene and a 1,1‘-Diphosphaferrocene
Plażuk, Damian; Kłys, Arkadiusz; Zakrzewski, Janusz; Rybarczyk-Pirek, Agnieszka; Olszak, Tomasz A.; Organometallics 20 (2001) 4448–; doi:10.1021/om010413o

data_4077376
_publ_section_title
;
 Direct Acetoacetylation of Ferrocene and a 1,1&#x2018;-Diphosphaferrocene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4448
_journal_paper_doi               10.1021/om010413o
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C14 H13 B F2 Fe O2'
_chemical_formula_weight         317.90
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.341(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5020(5)
_cell_length_b                   10.1884(5)
_cell_length_c                   12.8778(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.02
_cell_measurement_theta_min      27.46
_cell_volume                     1328.81(11)
_computing_cell_refinement       'MSC/AFC Molecular Control Software (1989a)'
_computing_data_collection       'MSC/AFC Molecular Control Software (1989a)'
_computing_data_reduction        'TEXSAN (1989b)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'AFC5S Rigaku'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2691
_diffrn_reflns_theta_full        72.66
_diffrn_reflns_theta_max         72.66
_diffrn_reflns_theta_min         4.37
_diffrn_standards_decay_%        <1.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.305
_exptl_absorpt_correction_T_max  0.6522
_exptl_absorpt_correction_T_min  0.2173
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'analytical from crystal shape (De Meulenaer, Tompa 1965)'
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.058P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                1374
_reflns_number_total             2546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010413o.cif
_cod_data_source_block           comp_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.058P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.058P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077376