Thioether-Functionalized Ferrocenyl-bis(phosphonite), Fe{(C5H4)P(−OC10H6(μ-S)C10H6O−)}2: Synthesis, Coordination Behavior, and Application in Suzuki-Miyaura Cross-Coupling Reactions
Punji, Benudhar; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic Chemistry 46 (2007) 10268–10275; doi:10.1021/ic701537k

data_4333474
_publ_section_title
;
 Thioether-Functionalized Ferrocenyl-bis(phosphonite),
 Fe{(C5H4)P(&#x2212;OC10H6(\m-S)C10H6O&#x2212;)}2:&#x00A0; Synthesis,
 Coordination Behavior, and Application in Suzuki-Miyaura Cross-Coupling
 Reactions
;
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10268
_journal_page_last               10275
_journal_paper_doi               10.1021/ic701537k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C53 H35 Cu2 Fe I2 N1.5 O6 P2 S2'
_chemical_formula_weight         1351.62
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.241(1)
_cell_angle_beta                 77.666(1)
_cell_angle_gamma                74.859(1)
_cell_formula_units_Z            2
_cell_length_a                   11.356(1)
_cell_length_b                   12.034(1)
_cell_length_c                   19.243(2)
_cell_measurement_reflns_used    8660
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.57
_cell_volume                     2479.7(4)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44145
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.8562
_exptl_absorpt_correction_T_min  0.7467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.980
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         12212
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+4.7558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                9624
_reflns_number_total             12212
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic701537ksup1.cif
_cod_data_source_block           msb285
_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 2.4.2 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      P-1
_cod_original_formula_sum        'C53 H35 Cu2 Fe I2 N1.50 O6 P2 S2'
_cod_database_code               4333474