Studies of how redox chemistry influences the synthesis of transition metal phosphametallocenes: a convenient synthesis of 2,5-diester-substituted phosphametallocenes and 2,2′,5,5′-tetraester-substituted-1,1′-diphosphaferrocenes
Carmichael, Duncan; Le Goff, Xavier F.; Muller, Eric; New Journal of Chemistry 34 (2010) 1341–; doi:10.1039/b9nj00440h

data_7053316
_publ_section_title
;
 Studies of how redox chemistry influences the synthesis of transition
 metal phosphametallocenes: a convenient synthesis of
 2,5-diester-substituted phosphametallocenes and
 2,2&#x2032;,5,5&#x2032;-tetraester-substituted-1,1&#x2032;-diphosphaferrocenes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1341
_journal_paper_doi               10.1039/b9nj00440h
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C20 H24 Fe O8 P2'
_chemical_formula_sum            'C20 H24 Fe O8 P2'
_chemical_formula_weight         510.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2c'
_symmetry_space_group_name_H-M   'C c m 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.473(1)
_cell_length_b                   21.153(1)
_cell_length_c                   13.311(1)
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2104.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7674
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.8825
_exptl_absorpt_correction_T_min  0.7708
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.142(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0329P)^2^+0.3328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                2322
_reflns_number_total             2535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00440h.txt
_cod_data_source_block           em371b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'Ccm21 '
_cod_database_code               7053316