Pentacarbonyl(3,3',4,4'-tetramethyl-1,1'-diphosphaferrocene-κ<i>P</i>)tungsten(0)
Sieroń, Lesław; Tosik, Anita; Acta Crystallographica Section E 60 (2004) m1828–m1829; doi:10.1107/S1600536804028910

data_2204755
_publ_section_title
Pentacarbonyl(3,3',4,4'-tetramethyl-1,1'-diphosphaferrocene-\k<i>P</i>)tungsten(0)
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1828
_journal_page_last               m1829
_journal_paper_doi               10.1107/S1600536804028910
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[W Fe (C6 H8 P)2 (C O)5]'
_chemical_formula_moiety         'C17 H16 Fe O5 P2 W'
_chemical_formula_sum            'C17 H16 Fe O5 P2 W'
_chemical_formula_weight         601.93
_chemical_name_systematic
;
Pentacarbonyl(3,3',4,4'-tetramethyl-1,1'-diphosphaferrocene-\kP)tungsten(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 101.02(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.279(13)
_cell_length_b                   10.857(9)
_cell_length_c                   14.061(12)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      3.6
_cell_volume                     1990(3)
_computing_cell_refinement       'P3 Software'
_computing_data_collection       'P3 Software (Siemens, 1993)'
_computing_data_reduction        'XDISK in SHELXTL/PC (Sheldrick, 1990)'
_computing_molecular_graphics    'XP in SHELXTL/PC'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P3'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4752
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.689
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.674
_refine_ls_extinction_coef       0.00038(9)
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0306P)^2^+1.1109P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                3802
_reflns_number_total             4567
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nc6008.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204755