Synthesis, structure and reactivity of ferrio-chloro-phosphanes, -arsanes and -stibanes [(CO)2(eta5-C5Me5)FePn(Cl)R] (Pn = P, As, Sb); R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl, 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes.
Weber, Lothar; Pumpenmeier, Lars; Stammler, Hans-Georg; Neumann, Beate; Dalton transactions (Cambridge, England : 2003)  (2004) 659–667; doi:10.1039/b315221a

data_7013838
_publ_section_title
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 Synthesis, structure and reactivity of ferrio-chloro-phosphanes,
 -arsanes and -stibanes [(CO)2(eta5-C5Me5)FePn(Cl)R] (Pn = P, As, Sb);
 R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl,
 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel
 metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              659
_journal_page_last               667
_journal_paper_doi               10.1039/b315221a
_journal_year                    2004
_chemical_formula_moiety         'C54 H65 Fe O2 Sb'
_chemical_formula_sum            'C54 H65 Fe O2 Sb'
_chemical_formula_weight         923.66
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.8230(5)
_cell_angle_beta                 73.7590(4)
_cell_angle_gamma                72.1330(5)
_cell_formula_units_Z            2
_cell_length_a                   10.34100(10)
_cell_length_b                   15.21400(10)
_cell_length_c                   16.2210(2)
_cell_measurement_reflns_used    13518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     2322.43(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD '
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            95916
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.9125
_exptl_absorpt_correction_T_min  0.8883
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.097
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         13551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0443P)^2^+2.3569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                12003
_reflns_number_total             13551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315221a.txt
_cod_data_source_block           compound7c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               7013838