Cyclotriphosphorus Complexes: Solid-State Structures and Dynamic Behavior of Monoadducts with Carbonyl Fragments
Massimo Di Vaira; Markus P. Ehses; Piero Stoppioni; Maurizio Peruzzini; Inorganic Chemistry 39 (2000) 2199–2205; doi:10.1021/ic991380w

data_4320958
_publ_contact_author
;
  Prof. P. Stoppioni
  Dipartimento di Chimica
  via Maragliano 77
  50144 Firenze
  Italy
;
_publ_contact_author_email       stopmora@chim1.unifi.it
_publ_contact_author_fax         '++39 055 354845'
_publ_contact_author_phone       '++39 055 3216328'
_publ_section_title
;
 Cyclotriphosphorus Complexes: Solid-State Structures and Dynamic Behavior
 of Monoadducts with Carbonyl Fragments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2199
_journal_page_last               2205
_journal_paper_doi               10.1021/ic991380w
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C53 H47 B Co F4 O5 P6 Re'
_chemical_formula_weight         1281.66
_chemical_name_systematic
;
[{1,1,1-tris(diphenylphosphinomethyl)ethane
cobalt}(=B5,h3:1-cyclotriphosphorus)
(rhenium pentacarbonyl)]tetrafluoroborate
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.754(2)
_cell_length_b                   24.886(4)
_cell_length_c                   15.182(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      57.5
_cell_measurement_theta_min      3.5
_cell_volume                     5423.0(14)
_computing_cell_refinement       'SAINT (Bruker-AXS software'
_computing_data_collection       'SMART (Bruker-AXS software'
_computing_data_reduction        'SAINT (Bruker-AXS software'
_computing_molecular_graphics    'ORTEP (C.K. Johnson)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92/SIR97 (Giacovazzo et al.)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CCD Bruker-AXS platform'
_diffrn_radiation_monochromator  'Goebel mirrors'
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19188
_diffrn_reflns_theta_max         57.46
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    8.87
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.649
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.900
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_reflns         7089
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.900
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_obs          0.0529
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_obs         0.1228
_reflns_number_observed          4688
_reflns_number_total             7089
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991380w_1.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] 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^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5423.0(13)
_cod_database_code               4320958