Tetra- and Decanuclear Iron(III) Phosphonates: Observance of a Rare P-C Bond Cleavage in a Homogeneous Medium
Ramaswamy Murugavel; Nayanmoni Gogoi; Rodolphe Clérac; Inorganic Chemistry 48 (2009) 646–651; doi:10.1021/ic8017562

data_4301233
_publ_contact_author_address
;
Department of Chemistry
Indian Institute of Technology Bombay
Powai
Mumbai
Maharastra
400076
INDIA
;
_publ_contact_author_email       RMV@CHEM.IITB.AC.IN
_publ_contact_author_name        'Ramaswamy Murugavel'
_publ_section_title
;
Tetra- and Decanuclear Iron(III) Phosphonates: Observance of a Rare P-C
Bond Cleavage in a Homogeneous Medium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              646
_journal_page_last               651
_journal_paper_doi               10.1021/ic8017562
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C65.5 H74.5 Cl1 Fe4 N6.5 O16 P3'
_chemical_formula_sum            'C65.5 H74.5 Cl Fe4 N6.5 O16 P3'
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_chemical_name_systematic
;
 ?
;
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_cell_angle_beta                 91.594(2)
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_cell_length_a                   14.7362(4)
_cell_length_b                   25.4076(6)
_cell_length_c                   20.3945(5)
_cell_measurement_reflns_used    20374
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_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.997
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_diffrn_measurement_details
;
  1 omega  -51.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908  -75.0000  240.0000    0.0000    0.0000 53

  2 omega  -51.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908  -75.0000    0.0000    0.0000    0.0000 53

  3 omega -100.00  -47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908  -75.0000    0.0000    0.0000    0.0000 53

  4 phi    118.00  180.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -29.1908    0.0000     -        0.0000    0.0000 62

  5 omega  -52.00   -7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908   75.0000  120.0000    0.0000    0.0000 45

  6 omega  -42.00  -14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -45.0000    0.0000    0.0000    0.0000 28

  7 omega    9.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000  120.0000    0.0000    0.0000 52

  8 omega  -43.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -45.0000  120.0000    0.0000    0.0000 51

  9 omega    2.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   45.0000    0.0000    0.0000    0.0000 42

 10 omega  -30.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  130.0000  236.0000    0.0000    0.0000 28

 11 omega  -43.00   10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000  120.0000    0.0000    0.0000 53

 12 omega   51.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   45.0000  240.0000    0.0000    0.0000 50

 13 omega   63.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   75.0000  240.0000    0.0000    0.0000 28

 14 omega    8.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -45.0000  120.0000    0.0000    0.0000 49

;
_diffrn_measurement_device_type  'OXFORD DIFFRACTIOM X CALIBUR-S'
_diffrn_measurement_method       'omega(w)-q scan'
_diffrn_orient_matrix_UB_11      -0.0110120310
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_diffrn_orient_matrix_UB_13      -0.0200243095
_diffrn_orient_matrix_UB_21      0.0154884557
_diffrn_orient_matrix_UB_22      -0.0170560270
_diffrn_orient_matrix_UB_23      0.0256041575
_diffrn_orient_matrix_UB_31      -0.0444202488
_diffrn_orient_matrix_UB_32      -0.0004643725
_diffrn_orient_matrix_UB_33      0.0128427880
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
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_diffrn_reflns_theta_full        25.00
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_exptl_absorpt_correction_type   multi-scan
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;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3228
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.069
_refine_diff_density_min         -2.154
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         13412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0982
_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^)+(0.1017P)^2^+61.9267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2668
_reflns_number_gt                8838
_reflns_number_total             13412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017562_si_001_2.cif
_cod_data_source_block           newrm175relabeled
_cod_original_formula_sum        'C65.50 H74.50 Cl Fe4 N6.50 O16 P3'
_cod_database_code               4301233