Imidazole Phosphines: Synthesis, Reaction Chemistry, and Their Use in SuzukiC,CCross-Coupling Reactions
Milde, Bianca; Packheiser, Rico; Hildebrandt, Stefanie; Schaarschmidt, Dieter; Rüffer, Tobias; Lang, Heinrich; Organometallics 31 (2012) 3661–; doi:10.1021/om300145d

data_4083280
_publ_section_title
;
 Imidazole Phosphines: Synthesis, Reaction Chemistry, and Their Use in
 SuzukiC,CCross-Coupling Reactions
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3661
_journal_paper_doi               10.1021/om300145d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C148 H112 Cl4 Fe2 P8 Pt4, 11(C H Cl3)'
_chemical_formula_sum            'C159 H123 Cl37 Fe2 P8 Pt4'
_chemical_formula_weight         4485.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_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                 102.178(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.4813(7)
_cell_length_b                   10.8030(5)
_cell_length_c                   34.7075(9)
_cell_measurement_reflns_used    4373
_cell_measurement_temperature    100
_cell_measurement_theta_max      61.9982
_cell_measurement_theta_min      3.5481
_cell_volume                     8606.1(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_sigmaI/netI    0.1976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            26442
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         4.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    13.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
During the measurement at 100 K the crystals were loosing CHCl3 as packing solvent, affecting thereby the crystal quality. Rapid measurements were performed to avoid this process as much as possible, however, a reasonable data collection was only possible up to a completeness of aprox. 85%.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4380
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.745
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         11727
_refine_ls_number_restraints     520
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2224
_reflns_number_gt                5676
_reflns_number_total             11727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            stef07.cif
_cod_data_source_block           stef07
_cod_original_sg_symbol_H-M      'P1 2/n 1'
_cod_database_code               4083280