#------------------------------------------------------------------------------
#$Date: 2025-08-04 10:03:09 +0300 (Mon, 04 Aug 2025) $
#$Revision: 301442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/67/7056707.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7056707
loop_
_publ_author_name
'Lee, Sze-Ling'
'Hu, Fei-long'
'Shang, Xiu-Juan'
'Shi, Yi-Xiang'
'Tan, Ai Ling'
'Mizera, Jens'
'Clegg, Jack Kay'
'Zhang, Wen-Hua'
'Young, David James'
'Lang, Jian-Ping'
_publ_section_title
;
 Efficient ring-opening polymerization (ROP) of ɛ-caprolactone
 catalysed by isomeric pyridyl β-diketonate iron(lll) complexes
;
_journal_issue                   23
_journal_name_full               'New J. Chem.'
_journal_page_first              14457
_journal_page_last               14465
_journal_paper_doi               10.1039/C7NJ03571C
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         '(C39 H27 Fe N6 O6), 0.5(H2 O)'
_chemical_formula_sum            'C39 H28 Fe N6 O6.5'
_chemical_formula_weight         740.52
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.2613(7)
_cell_length_b                   14.2613(7)
_cell_length_c                   30.489(2)
_cell_measurement_reflns_used    1483
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4910
_cell_measurement_theta_min      3.5590
_cell_volume                     5370.2(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            4761
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.857
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       Block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0751
_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/[σ²(Fo²)+(0.1627P)²+10.5326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2468
_refine_ls_wR_factor_ref         0.2725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1503
_reflns_number_total             2104
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj03571c1.cif
_cod_data_source_block           CPX1
_cod_original_cell_volume        5370.2(6)
_cod_original_formula_sum        'C39 H28 Fe N6 O6.50'
_cod_database_code               7056707
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.915
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.3333 0.6667 0.06400(4) 0.0424(5) Uani 1 3 d S T P . .
O1 O 0.2556(3) 0.5382(3) 0.02463(11) 0.0515(10) Uani 1 1 d . . . . .
O1W O 0.0000 0.0000 -0.0480(4) 0.088(5) Uani 0.5 3 d S T P . .
H1W H -0.0003 -0.0538 -0.0375 0.106 Uiso 0.3333 1 d R U P . .
O2 O 0.2001(3) 0.6017(3) 0.10047(10) 0.0439(9) Uani 1 1 d . . . . .
C13 C -0.0873(4) 0.4426(4) 0.11144(18) 0.0645(15) Uani 0.3333 1 d . . P A 1
H13 H -0.1052 0.4049 0.0850 0.077 Uiso 0.3333 1 calc R U P A 1
N2 N -0.1646(5) 0.4266(5) 0.1403(2) 0.0793(19) Uani 0.3333 1 d . . P A 1
N2A N -0.0873(4) 0.4426(4) 0.11144(18) 0.0645(15) Uani 0.6667 1 d . . P A 2
C13A C -0.1646(5) 0.4266(5) 0.1403(2) 0.0793(19) Uani 0.6667 1 d . . P A 2
H13A H -0.2361 0.3763 0.1336 0.095 Uiso 0.6667 1 calc R U P A 2
N1 N 0.0112(5) 0.3357(5) -0.02610(17) 0.0667(17) Uani 0.3333 1 d . . P B 1
C1 C -0.0204(6) 0.2735(6) -0.0634(2) 0.094(2) Uani 0.3333 1 d . . P B 1
H1 H -0.0932 0.2246 -0.0685 0.113 Uiso 0.3333 1 calc R U P B 1
C1A C 0.0112(5) 0.3357(5) -0.02610(17) 0.0667(17) Uani 0.6667 1 d . . P B 2
H1A H -0.0401 0.3292 -0.0056 0.080 Uiso 0.6667 1 calc R U P B 2
N1A N -0.0204(6) 0.2735(6) -0.0634(2) 0.094(2) Uani 0.6667 1 d . . P B 2
C2 C 0.0557(6) 0.2842(6) -0.0928(2) 0.079(2) Uani 1 1 d . . . . .
H2 H 0.0338 0.2412 -0.1178 0.095 Uiso 1 1 calc R U . B 1
C3 C 0.1636(6) 0.3559(7) -0.0870(2) 0.084(2) Uani 1 1 d . . . . .
H3 H 0.2146 0.3616 -0.1074 0.101 Uiso 1 1 calc R U . . .
C4 C 0.1937(5) 0.4183(6) -0.0504(2) 0.074(2) Uani 1 1 d . . . . .
H4 H 0.2661 0.4697 -0.0461 0.089 Uiso 1 1 calc R U . . .
C5 C 0.1170(5) 0.4062(5) -0.01936(16) 0.0506(13) Uani 1 1 d . . . . .
C6 C 0.1530(4) 0.4776(4) 0.02049(15) 0.0438(12) Uani 1 1 d . . . . .
C7 C 0.0776(4) 0.4731(5) 0.05034(17) 0.0499(13) Uani 1 1 d . . . . .
H7 H 0.0048 0.4272 0.0441 0.060 Uiso 1 1 calc R U . . .
C8 C 0.1035(4) 0.5325(4) 0.08892(15) 0.0411(11) Uani 1 1 d . . . . .
C9 C 0.0166(4) 0.5139(4) 0.12111(16) 0.0431(12) Uani 1 1 d . . . . .
C10 C 0.0420(5) 0.5686(5) 0.16082(17) 0.0558(15) Uani 1 1 d . . . . .
H10 H 0.1139 0.6167 0.1679 0.067 Uiso 1 1 calc R U . . .
C11 C -0.0385(5) 0.5521(5) 0.18973(19) 0.0636(16) Uani 1 1 d . . . . .
H11 H -0.0220 0.5891 0.2163 0.076 Uiso 1 1 calc R U . . .
C12 C -0.1432(5) 0.4804(5) 0.1788(2) 0.0700(18) Uani 1 1 d . . . . .
H12 H -0.1993 0.4686 0.1977 0.084 Uiso 1 1 calc R U . A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Fe1 O2 91.71(13) . 3_565
O2 Fe1 O2 91.71(13) . 2_665
O2 Fe1 O2 91.70(13) 3_565 2_665
O2 Fe1 O1 93.88(15) . 3_565
O2 Fe1 O1 86.91(14) 3_565 3_565
O2 Fe1 O1 174.29(14) 2_665 3_565
O2 Fe1 O1 174.28(14) . 2_665
O2 Fe1 O1 93.88(15) 3_565 2_665
O2 Fe1 O1 86.91(14) 2_665 2_665
O1 Fe1 O1 87.65(15) 3_565 2_665
O2 Fe1 O1 86.91(14) . .
O2 Fe1 O1 174.29(14) 3_565 .
O2 Fe1 O1 93.88(15) 2_665 .
O1 Fe1 O1 87.65(15) 3_565 .
O1 Fe1 O1 87.65(15) 2_665 .
C6 O1 Fe1 127.0(3) . .
C8 O2 Fe1 128.0(3) . .
N2 C13 C9 119.1(5) . .
N2 C13 H13 120.4 . .
C9 C13 H13 120.4 . .
C13 N2 C12 122.8(6) . .
C13A N2A C9 119.1(5) . .
N2A C13A C12 122.8(6) . .
N2A C13A H13A 118.6 . .
C12 C13A H13A 118.6 . .
C5 N1 C1 119.5(6) . .
C2 C1 N1 119.2(6) . .
C2 C1 H1 120.4 . .
N1 C1 H1 120.4 . .
C5 C1A N1A 119.5(6) . .
C5 C1A H1A 120.3 . .
N1A C1A H1A 120.3 . .
C2 N1A C1A 119.2(6) . .
N1A C2 C3 122.5(6) . .
C1 C2 C3 122.5(6) . .
C1 C2 H2 118.8 . .
C3 C2 H2 118.8 . .
C4 C3 C2 117.8(6) . .
C4 C3 H3 121.1 . .
C2 C3 H3 121.1 . .
C3 C4 C5 120.5(6) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C1A C5 C4 120.5(5) . .
N1 C5 C4 120.5(5) . .
C1A C5 C6 120.4(5) . .
N1 C5 C6 120.4(5) . .
C4 C5 C6 119.1(5) . .
O1 C6 C7 124.4(4) . .
O1 C6 C5 115.2(4) . .
C7 C6 C5 120.4(5) . .
C6 C7 C8 124.5(5) . .
C6 C7 H7 117.8 . .
C8 C7 H7 117.8 . .
O2 C8 C7 124.0(5) . .
O2 C8 C9 115.7(4) . .
C7 C8 C9 120.3(5) . .
N2A C9 C10 119.7(5) . .
C13 C9 C10 119.7(5) . .
N2A C9 C8 119.4(4) . .
C13 C9 C8 119.4(4) . .
C10 C9 C8 120.8(5) . .
C11 C10 C9 120.3(6) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C12 C11 C10 118.7(5) . .
C12 C11 H11 120.7 . .
C10 C11 H11 120.7 . .
C13A C12 C11 119.4(6) . .
N2 C12 C11 119.4(6) . .
N2 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 1.986(3) .
Fe1 O2 1.986(3) 3_565
Fe1 O2 1.986(3) 2_665
Fe1 O1 1.999(3) 3_565
Fe1 O1 1.999(3) 2_665
Fe1 O1 1.999(3) .
O1 C6 1.280(6) .
O1W H1W 0.8300 .
O2 C8 1.280(6) .
C13 N2 1.338(8) .
C13 C9 1.345(7) .
C13 H13 0.9300 .
N2 C12 1.350(9) .
N2A C13A 1.338(8) .
N2A C9 1.345(7) .
C13A C12 1.350(9) .
C13A H13A 0.9300 .
N1 C5 1.346(8) .
N1 C1 1.373(8) .
C1 C2 1.355(9) .
C1 H1 0.9300 .
C1A C5 1.346(8) .
C1A N1A 1.373(8) .
C1A H1A 0.9300 .
N1A C2 1.355(9) .
C2 C3 1.367(10) .
C2 H2 0.9300 .
C3 C4 1.355(8) .
C3 H3 0.9300 .
C4 C5 1.390(8) .
C4 H4 0.9300 .
C5 C6 1.501(7) .
C6 C7 1.386(7) .
C7 C8 1.387(7) .
C7 H7 0.9300 .
C8 C9 1.497(7) .
C9 C10 1.387(7) .
C10 C11 1.371(8) .
C10 H10 0.9300 .
C11 C12 1.364(9) .
C11 H11 0.9300 .
C12 H12 0.9300 .
