Phosphinoferrocene Ureas: Synthesis, Structural Characterization, and Catalytic Use in Palladium-Catalyzed Cyanation of Aryl Bromides
Škoch, Karel; Císařová, Ivana; Štěpnička, Petr; Organometallics 34 (2015) 1942–; doi:10.1021/acs.organomet.5b00197

data_4085821
_publ_section_title
;
 Phosphinoferrocene Ureas: Synthesis, Structural Characterization, and
 Catalytic Use in Palladium-Catalyzed Cyanation of Aryl Bromides
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1942
_journal_paper_doi               10.1021/acs.organomet.5b00197
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C23 H23 Fe N P, Cl'
_chemical_formula_sum            'C23 H23 Cl Fe N P'
_chemical_formula_weight         435.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.4731(7)
_cell_length_b                   6.0911(2)
_cell_length_c                   27.5242(9)
_cell_measurement_reflns_used    5589
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.37
_cell_volume                     4103.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27344
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.943
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+20.7259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                6368
_reflns_number_total             8063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00197_si_002.cif
_cod_data_source_block           ks80
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity' tag as specified in the
replacement file
'/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3376 2015-05-07 07:48:27Z andrius 

 Adding full bibliography for 4085821--4085828.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085821