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_7038344
_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         'C34 H30 B2 Cl F2 Fe N6 O8 P S, 2(C H Cl2)'
_chemical_formula_sum            'C36 H34 B2 Cl5 F2 Fe N6 O8 P S'
_chemical_formula_weight         1034.44
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-18
_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                90
_cell_formula_units_Z            4
_cell_length_a                   15.441(2)
_cell_length_b                   16.407(2)
_cell_length_c                   17.367(2)
_cell_measurement_reflns_used    9020
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.16
_cell_volume                     4399.8(9)
_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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.765
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane '
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8621
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+32.1919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5649
_reflns_number_total             8621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00164e2.cif
_cod_data_source_block           od2
_cod_depositor_comments
'Adding full bibliography for 7038343--7038346.cif.'
_cod_original_cell_volume        4399.8(10)
_cod_database_code               7038344
_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
 C31A-C32A = C31B-C32B = C33A-C34A = C33B-C34B
 1.5 with sigma of 0.005
 O8A-C33A \\sim O8B-C33B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(B1) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uiso(O8A) = Uiso(C33A) = Uiso(C34A)
Uiso(O8B) = Uiso(C33B) = Uiso(C34B)
Uiso(C32A) = Uiso(C32B)
Uanis(C15) = Uanis(C16) = Uanis(C17)
4. Others
 Fixed Sof: C31A(0.5) H31A(0.5) H31B(0.5) C32A(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) S1A(0.5) O8A(0.5) C33A(0.5) H33A(0.5) H33B(0.5) C34A(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) S1B(0.5) C31B(0.5) H31C(0.5) H31D(0.5) C32B(0.5) H32D(0.5)
 H32E(0.5) H32F(0.5) O8B(0.5) C33B(0.5) H33C(0.5) H33D(0.5) C34B(0.5) H34D(0.5)
 H34E(0.5) H34F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C33A(H33A,H33B), C31B(H31C,H31D), C33B(H33C,H33D)
5.b Me refined with riding coordinates:
 C32A(H32A,H32B,H32C), C34A(H34A,H34B,H34C), C32B(H32D,H32E,H32F)
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:
 C34B(H34D,H34E,H34F)
;
_shelx_res_checksum              11115
_shelx_fab_checksum              90687
_olex2_submission_special_instructions 'No special instructions were received'