Clathrochelates meet phosphorus: thiophosphorylation of Fe(ii) dichloroclathrochelate precursor, synthesis of N,S-donor macrobicyclic ligands and their Pd(ii) complexes as potent catalysts of Suzuki cross-coupling reaction.
Artyushin, Oleg I.; Odinets, Irina L.; Matveeva, Ekaterina V.; Vologzhanina, Anna V.; Varzatskii, Oleg A.; Lyubimov, Sergey E.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9677–9689; doi:10.1039/c3dt53590h

data_7030964
_publ_section_title
;
 Clathrochelates meet phosphorus: thiophosphorylation of Fe(ii)
 dichloroclathrochelate precursor, synthesis of N,S-donor macrobicyclic
 ligands and their Pd(ii) complexes as potent catalysts of Suzuki
 cross-coupling reaction.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9677
_journal_page_last               9689
_journal_paper_doi               10.1039/c3dt53590h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C49 H38 B2 Cl F2 Fe N8 O6 P Pd S, 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H42 B2 Cl5 F2 Fe N8 O6 P Pd S'
_chemical_formula_weight         1325.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.3940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7464(10)
_cell_length_b                   12.4506(7)
_cell_length_c                   27.3672(15)
_cell_measurement_reflns_used    648
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.43
_cell_volume                     5689.4(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detetor'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44435
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.157
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         11132
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+50.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7276
_reflns_number_total             11132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53590h2.cif
_cod_data_source_block           6d
_cod_depositor_comments
'Adding full bibliography for 7030958--7030964.cif.'
_cod_database_code               7030964
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.787
_shelx_res_checksum              79433