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_7038343
_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         'C42 H30 B2 Cl F2 Fe N6 O7 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C44 H35 B2 Cl F2 Fe N6 O7.5 P'
_chemical_formula_weight         949.67
_chemical_name_systematic
;
 ? 
;
_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   mixed
_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                116.261(3)
_cell_angle_beta                 91.671(3)
_cell_angle_gamma                95.321(4)
_cell_formula_units_Z            2
_cell_length_a                   12.3200(13)
_cell_length_b                   13.7730(18)
_cell_length_c                   13.8321(17)
_cell_measurement_reflns_used    2170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.80
_cell_measurement_theta_min      2.21
_cell_volume                     2089.3(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_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    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24879
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.647
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABs (Sheldrick, 1998)'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether/hexane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         11049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.2451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8961
_reflns_number_total             11049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00164e2.cif
_cod_data_source_block           od4
_cod_depositor_comments
'Adding full bibliography for 7038343--7038346.cif.'
_cod_original_formula_sum        'C44 H35 B2 Cl F2 Fe N6 O7.50 P'
_cod_database_code               7038343
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.835
_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. Others
 Fixed Sof: O1S(0.5) C1SA(0.5) H1SA(0.5) H1SB(0.5) C2SA(0.5) H2SA(0.5)
 H2SB(0.5) H2SC(0.5) C1SB(0.5) H1SC(0.5) H1SD(0.5) C2SB(0.5) H2SD(0.5)
 H2SE(0.5) H2SF(0.5)
3.a Riding coordinates:
 C1SA(H1SA,H1SB), C1SB(H1SC,H1SD)
3.b Me refined with riding coordinates:
 C2SA(H2SA,H2SB,H2SC), C2SB(H2SD,H2SE,H2SF)
3.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), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              73453
_olex2_submission_special_instructions 'No special instructions were received'