Clathrochelates meet phosphorus. New thio- and phosphorylation reactions of an iron(ii) dichloroclathrochelate precursor and preparation of its first phosphorus(iii)-containing macrobicyclic derivative.
Artyushin, Oleg I.; Matveeva, Ekaterina V.; Vologzhanina, Anna V.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5328–5333; doi:10.1039/c6dt00164e

data_7038345
_publ_section_title
;
 Clathrochelates meet phosphorus. New thio- and phosphorylation reactions
 of an iron(ii) dichloroclathrochelate precursor and preparation of its
 first phosphorus(iii)-containing macrobicyclic derivative.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5328
_journal_page_last               5333
_journal_paper_doi               10.1039/c6dt00164e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C38 H40 B2 F2 Fe N6 O10 P2 S2, 0.75(C6 H14)'
_chemical_formula_sum            'C48.5 H64.5 B2 F2 Fe N6 O10 P2 S2'
_chemical_formula_weight         1133.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-18 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   38.5967(16)
_cell_length_b                   38.5967(16)
_cell_length_c                   23.9936(15)
_cell_measurement_reflns_used    1456
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.781
_cell_measurement_theta_min      2.453
_cell_volume                     30955(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            79579
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.514
_diffrn_reflns_theta_min         2.267
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Shelcdrick, 1998)''
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       plate
_exptl_crystal_F_000             10683
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/heptane'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The asymmetric unit contains three independent solvate hexane molecules, two 
with partial occupancies and strongly disordered third one. The latter 
molecule have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON using ABIN instruction. 
Chemical formula, formula 
weight and Dx were calculated taking the solvate molecules into account.
;
_refine_diff_density_max         1.316
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         12025
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+69.7276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9865
_reflns_number_total             12025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00164e2.cif
_cod_data_source_block           od15
_cod_depositor_comments
'Adding full bibliography for 7038343--7038346.cif.'
_cod_original_formula_sum        'C48.50 H64.50 B2 F2 Fe N6 O10 P2 S2'
_cod_database_code               7038345
_shelxl_version_number           2014-3
_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. Restrained distances
 C35-C36A = C7S-C8S = C11S-C12S
 1.5 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C36) = Uanis(C36A)
Uanis(C37) = Uanis(C38)
Uanis(C33) = Uanis(C34)
Uanis(C6S) = Uanis(C5S) = Uanis(C4S) = Uanis(C3S) = Uanis(C2S) = Uanis(C1S)
Uanis(C12S) = Uanis(C11S) = Uanis(C10S) = Uanis(C9S) = Uanis(C8S) = Uanis(C7S)
4. Others
 Fixed Sof: C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36A(0.5) H36D(0.5)
 H36E(0.5) H36F(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) C7S(0.25)
 H7SA(0.25) H7SB(0.25) H7SC(0.25) C8S(0.25) H8SA(0.25) H8SB(0.25) C9S(0.25)
 H9SA(0.25) H9SB(0.25) C10S(0.25) H10A(0.25) H10B(0.25) C11S(0.25) H11A(0.25)
 H11B(0.25) C12S(0.25) H12A(0.25) H12B(0.25) H12C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C2S(H2SA,
 H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C8S(H8SA,H8SB),
 C9S(H9SA,H9SB), C10S(H10A,H10B), C11S(H11A,H11B)
5.b Me refined with riding coordinates:
 C36A(H36D,H36E,H36F), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC), C7S(H7SA,H7SB,
 H7SC), C12S(H12A,H12B,H12C)
5.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)
5.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              76704
_shelx_fab_checksum              29176
_olex2_submission_special_instructions 'No special instructions were received'