#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:43:40 +0200 (lun 05 de jul de 2021) $
#$Revision: 267192 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/73/7707357.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_7707357
loop_
_publ_author_name
'Wang, Kuiyuan'
'Prior, Timothy J.'
'Hughes, David L.'
'Arbaoui, Abdessamad'
'Redshaw, Carl'
_publ_section_title
;
 Coordination chemistry of [2 + 2] Schiff-base macrocycles derived from
 the dianilines
 [(2-NH₂C₆H₄)₂X] (X =
 CH₂CH₂, O): structural studies and ROP capability
 towards cyclic esters.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8057
_journal_page_last               8069
_journal_paper_doi               10.1039/d1dt00711d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
; 
 C28 H32 Br2 Fe2 N2 O6, 2(C2 H3 N)
;
_chemical_formula_sum            'C32 H38 Br2 Fe2 N4 O6'
_chemical_formula_weight         846.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.2110(10)
_cell_angle_beta                 102.4660(10)
_cell_angle_gamma                97.4090(10)
_cell_formula_units_Z            1
_cell_length_a                   8.51990(10)
_cell_length_b                   9.20980(10)
_cell_length_c                   12.1881(2)
_cell_measurement_reflns_used    17670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0970
_cell_measurement_theta_min      3.8250
_cell_volume                     901.29(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Mercury, ORTEP'
_computing_publication_material  'SHELXL, ciftab'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32046
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.343
_diffrn_reflns_theta_min         3.816
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    9.433
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0509P)²+0.4803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3268
_reflns_number_total             3387
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_database_code               7707357
_shelx_shelxl_version_number     2018/3
_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   0.765
_shelx_estimated_absorpt_t_max   0.912
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.3821(3) 0.1102(2) 0.31993(18) 0.0220(4) Uani 1 1 d . . . . .
C2 C 0.3480(3) 0.2589(2) 0.33219(19) 0.0241(4) Uani 1 1 d . . . . .
C3 C 0.2944(3) 0.3175(3) 0.23453(19) 0.0257(5) Uani 1 1 d . . . . .
H3 H 0.2709(7) 0.420(3) 0.2466(4) 0.031 Uiso 1 1 calc R U . . .
C4 C 0.2735(3) 0.2362(3) 0.12264(19) 0.0250(5) Uani 1 1 d . . . . .
C5 C 0.3022(3) 0.0891(3) 0.11060(19) 0.0257(5) Uani 1 1 d . . . . .
H5 H 0.2858(6) 0.0306(19) 0.037(2) 0.031 Uiso 1 1 calc R U . . .
C6 C 0.3543(3) 0.0245(2) 0.20401(19) 0.0244(5) Uani 1 1 d . . . . .
C7 C 0.3596(3) 0.3584(2) 0.44154(19) 0.0257(5) Uani 1 1 d . . . . .
H7 H 0.3199(13) 0.451(3) 0.4385(2) 0.031 Uiso 1 1 calc R U . . .
C8 C 0.3725(3) -0.1308(2) 0.17296(19) 0.0255(5) Uani 1 1 d . . . . .
H8 H 0.3473(8) -0.1766(13) 0.090(2) 0.031 Uiso 1 1 calc R U . . .
C9 C 0.2160(3) 0.2981(3) 0.01526(19) 0.0270(5) Uani 1 1 d . . . . .
C10 C 0.2138(3) 0.4660(3) 0.0474(2) 0.0343(5) Uani 1 1 d . . . . .
H10A H 0.180069 0.502318 -0.022965 0.051 Uiso 1 1 calc R U . . .
H10B H 0.323406 0.519828 0.090419 0.051 Uiso 1 1 calc R U . . .
H10C H 0.136608 0.483925 0.095521 0.051 Uiso 1 1 calc R U . . .
C11 C 0.3324(3) 0.2723(3) -0.0643(2) 0.0357(6) Uani 1 1 d . . . . .
H11A H 0.331968 0.164325 -0.088187 0.054 Uiso 1 1 calc R U . . .
H11B H 0.443225 0.324259 -0.022732 0.054 Uiso 1 1 calc R U . . .
H11C H 0.296012 0.312024 -0.132691 0.054 Uiso 1 1 calc R U . . .
C12 C 0.0434(3) 0.2131(3) -0.0496(2) 0.0346(6) Uani 1 1 d . . . . .
H12A H -0.031292 0.228947 0.000768 0.052 Uiso 1 1 calc R U . . .
H12B H 0.045536 0.105388 -0.072041 0.052 Uiso 1 1 calc R U . . .
H12C H 0.005850 0.250719 -0.118817 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1596(3) 0.0229(3) 0.63178(19) 0.0295(5) Uani 1 1 d . . . . .
C14 C 0.0094(3) -0.0521(3) 0.6502(2) 0.0352(6) Uani 1 1 d . . . . .
H14A H -0.074082 0.011509 0.640877 0.053 Uiso 1 1 calc R U . . .
H14B H 0.030364 -0.069765 0.728341 0.053 Uiso 1 1 calc R U . . .
H14C H -0.029197 -0.148552 0.593653 0.053 Uiso 1 1 calc R U . . .
C15 C 0.2444(3) 0.6936(3) 0.7863(2) 0.0378(6) Uani 1 1 d . . . . .
C16 C 0.2290(4) 0.5621(3) 0.6942(3) 0.0494(7) Uani 1 1 d . . . . .
H16A H 0.226209 0.593232 0.621438 0.074 Uiso 1 1 calc R U . . .
H16B H 0.127877 0.492611 0.686474 0.074 Uiso 1 1 calc R U . . .
H16C H 0.322652 0.511712 0.712539 0.074 Uiso 1 1 calc R U . . .
N1 N 0.2746(3) 0.0799(2) 0.61470(17) 0.0305(4) Uani 1 1 d . . . . .
N2 N 0.2557(4) 0.7967(3) 0.8581(2) 0.0521(7) Uani 1 1 d . . . . .
O1 O 0.4150(2) 0.33858(17) 0.53948(13) 0.0273(3) Uani 1 1 d . . . . .
O2 O 0.43160(19) 0.05405(16) 0.40884(12) 0.0240(3) Uani 1 1 d . . . . .
O3 O 0.4158(2) -0.21324(17) 0.23818(13) 0.0276(3) Uani 1 1 d . . . . .
Fe1 Fe 0.51395(4) 0.16103(4) 0.58492(3) 0.02308(11) Uani 1 1 d . . . . .
Br1 Br 0.80745(3) 0.28365(3) 0.58613(2) 0.03222(10) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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
_geom_angle_publ_flag
O2 C1 C2 121.99(19) . . ?
O2 C1 C6 121.99(19) . . ?
C2 C1 C6 116.00(19) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 C7 115.0(2) . . ?
C1 C2 C7 123.9(2) . . ?
C4 C3 C2 122.8(2) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 116.1(2) . . ?
C3 C4 C9 123.6(2) . . ?
C5 C4 C9 120.2(2) . . ?
C4 C5 C6 123.6(2) . . ?
C4 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C5 C6 C1 120.4(2) . . ?
C5 C6 C8 114.97(19) . . ?
C1 C6 C8 124.7(2) . . ?
O1 C7 C2 127.6(2) . . ?
O1 C7 H7 116.2 . . ?
C2 C7 H7 116.2 . . ?
O3 C8 C6 127.9(2) . . ?
O3 C8 H8 116.1 . . ?
C6 C8 H8 116.1 . . ?
C10 C9 C12 109.6(2) . . ?
C10 C9 C4 111.61(19) . . ?
C12 C9 C4 108.70(19) . . ?
C10 C9 C11 108.4(2) . . ?
C12 C9 C11 109.1(2) . . ?
C4 C9 C11 109.39(19) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C14 178.3(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 179.7(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 N1 Fe1 171.5(2) . . ?
C7 O1 Fe1 128.99(15) . . ?
C1 O2 Fe1 129.84(13) . . ?
C1 O2 Fe1 129.71(13) . 2_656 ?
Fe1 O2 Fe1 99.86(6) . 2_656 ?
C8 O3 Fe1 128.48(14) . 2_656 ?
O1 Fe1 O3 105.97(6) . 2_656 ?
O1 Fe1 O2 85.85(6) . . ?
O3 Fe1 O2 166.12(6) 2_656 . ?
O1 Fe1 O2 164.53(6) . 2_656 ?
O3 Fe1 O2 87.20(6) 2_656 2_656 ?
O2 Fe1 O2 80.14(6) . 2_656 ?
O1 Fe1 N1 86.57(7) . . ?
O3 Fe1 N1 82.78(7) 2_656 . ?
O2 Fe1 N1 90.87(7) . . ?
O2 Fe1 N1 87.11(7) 2_656 . ?
O1 Fe1 Br1 92.75(5) . . ?
O3 Fe1 Br1 87.98(5) 2_656 . ?
O2 Fe1 Br1 98.88(5) . . ?
O2 Fe1 Br1 95.85(5) 2_656 . ?
N1 Fe1 Br1 170.16(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.302(3) . ?
C1 C2 1.422(3) . ?
C1 C6 1.431(3) . ?
C2 C3 1.413(3) . ?
C2 C7 1.439(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.98(3) . ?
C4 C5 1.393(3) . ?
C4 C9 1.537(3) . ?
C5 C6 1.400(3) . ?
C5 H5 0.93(3) . ?
C6 C8 1.445(3) . ?
C7 O1 1.243(3) . ?
C7 H7 0.96(3) . ?
C8 O3 1.234(3) . ?
C8 H8 0.99(3) . ?
C9 C10 1.523(3) . ?
C9 C12 1.536(3) . ?
C9 C11 1.538(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N1 1.130(3) . ?
C13 C14 1.456(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N2 1.137(4) . ?
C15 C16 1.453(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N1 Fe1 2.210(2) . ?
O1 Fe1 2.0488(16) . ?
O2 Fe1 2.1020(15) . ?
O2 Fe1 2.1035(15) 2_656 ?
O3 Fe1 2.0502(15) 2_656 ?
Fe1 Br1 2.6034(4) . ?
