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_7030961
_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         'C46 H40 B2 F2 Fe N7 O6 P S2, 2(C H Cl3)'
_chemical_formula_sum            'C48 H42 B2 Cl6 F2 Fe N7 O6 P S2'
_chemical_formula_weight         1236.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.13 svn.r2834 for OlexSys, GUI svn.r4705)
;
_cell_angle_alpha                90.88(4)
_cell_angle_beta                 100.76(3)
_cell_angle_gamma                112.68(5)
_cell_formula_units_Z            2
_cell_length_a                   13.219(14)
_cell_length_b                   13.73(2)
_cell_length_c                   16.225(18)
_cell_measurement_reflns_used    463
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.80
_cell_volume                     2657(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33841
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.70
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         16319
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0200P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                10825
_reflns_number_total             16319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53590h2.cif
_cod_data_source_block           od13
_cod_depositor_comments
'Adding full bibliography for 7030958--7030964.cif.'
_cod_original_cell_volume        2656(6)
_cod_database_code               7030961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Cl5A \\sim Cl5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl4A \\sim Cl4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C38 \\sim C38A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C39 \\sim C39A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C40 \\sim C40A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C41 \\sim C41A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C42 \\sim C42A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C37 \\sim C37A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uiso(C46) = Uiso(C46A)
Uanis(C36) = Uanis(C35) = Uanis(C34) = Uanis(C33) = Uanis(C32)
3. Others
 Fixed Sof: C37(0.75) C42(0.75) H42(0.75) C41(0.75) H41(0.75) C40(0.75)
 H40(0.75) C39(0.75) H39(0.75) C38(0.75) H38(0.75) C37A(0.25) C38A(0.25)
 H38A(0.25) C39A(0.25) H39A(0.25) C42A(0.25) H42A(0.25) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C46A(0.5) H46D(0.5) H46E(0.5) H46F(0.5) C40A(0.25)
 H40A(0.25) C41A(0.25) H41A(0.25) Cl4(0.75) Cl5(0.75) Cl4A(0.25) Cl5A(0.25)
4.a Ternary CH refined with riding coordinates:
 C2S(H2S), C1S(H1S)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C42(H42), C41(H41), C40(H40), C39(H39), C38(H38),
 C38A(H38A), C39A(H39A), C42A(H42A), C40A(H40A), C41A(H41A)
4.d Fitted hexagon refined as free rotating group:
 C37(C42,C41,C40,C39,C38)
4.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C46A(H46D,H46E,H46F)
;