#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:43:40 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707352.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_7707352
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
;
C12 H18 Fe N6, Br6 Fe2 O 
;
_chemical_formula_sum            'C12 H18 Br6 Fe3 N6 O'
_chemical_formula_weight         909.33
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.39520(10)
_cell_length_b                   12.39520(10)
_cell_length_c                   30.5277(3)
_cell_measurement_reflns_used    16669
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3390
_cell_measurement_theta_min      4.312
_cell_volume                     4061.92(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 
goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            24700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.751
_diffrn_reflns_theta_min         4.345
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    23.225
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.230
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0188
_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/[σ²(Fo²)+(0.0244P)²+13.9314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1639
_reflns_number_total             1644
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           FeROP12
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_original_cell_volume        4061.92(8)
_cod_database_code               7707352
_shelx_shelxl_version_number     2018/1
_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   0.123
_shelx_estimated_absorpt_t_max   0.562
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
Br1 Br 0.63880(2) 0.49656(2) 0.41810(2) 0.02042(9) Uani 1 1 d . . . . .
Br2 Br 0.80523(2) 0.84452(2) 0.41558(2) 0.02569(9) Uani 1 1 d . . . . .
Fe1 Fe 0.333333 0.666667 0.42514(2) 0.01390(14) Uani 1 3 d S T P . .
Fe2 Fe 0.666667 0.333333 0.39120(2) 0.01323(14) Uani 1 3 d S T P . .
Fe3 Fe 1.000000 1.000000 0.44226(2) 0.01377(14) Uani 1 3 d S T P . .
O1 O 0.666667 0.333333 0.333333 0.0257(9) Uani 1 6 d S T P . .
O2 O 1.000000 1.000000 0.500000 0.0328(11) Uani 1 6 d S T P . .
N2 N 0.33581(19) 0.52176(19) 0.38642(6) 0.0202(4) Uani 1 1 d . . . . .
N1 N 0.47681(18) 0.67239(18) 0.46684(6) 0.0185(4) Uani 1 1 d . . . . .
C1 C 0.5533(2) 0.6813(2) 0.48982(7) 0.0175(5) Uani 1 1 d . . . . .
C3 C 0.3342(2) 0.4371(2) 0.37136(7) 0.0193(5) Uani 1 1 d . . . . .
C2 C 0.6518(2) 0.6937(3) 0.51892(8) 0.0243(5) Uani 1 1 d . . . . .
H2A H 0.655384 0.742385 0.544737 0.036 Uiso 1 1 calc R U . . .
H2B H 0.731843 0.736264 0.503494 0.036 Uiso 1 1 calc R U . . .
H2C H 0.634665 0.610870 0.528150 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3324(3) 0.3282(2) 0.35223(8) 0.0249(5) Uani 1 1 d . . . . .
H4A H 0.291194 0.257628 0.372470 0.037 Uiso 1 1 calc R U . . .
H4B H 0.417971 0.346824 0.346955 0.037 Uiso 1 1 calc R U . . .
H4C H 0.286671 0.306996 0.324448 0.037 Uiso 1 1 calc R U . . .
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
N1 Fe1 N1 88.77(8) . 2_665 ?
N1 Fe1 N1 88.77(8) . 3_565 ?
N1 Fe1 N1 88.77(8) 2_665 3_565 ?
N1 Fe1 N2 89.77(7) . . ?
N1 Fe1 N2 176.84(8) 2_665 . ?
N1 Fe1 N2 88.40(7) 3_565 . ?
N1 Fe1 N2 88.40(7) . 2_665 ?
N1 Fe1 N2 89.78(7) 2_665 2_665 ?
N1 Fe1 N2 176.84(8) 3_565 2_665 ?
N2 Fe1 N2 92.99(8) . 2_665 ?
N1 Fe1 N2 176.84(8) . 3_565 ?
N1 Fe1 N2 88.40(7) 2_665 3_565 ?
N1 Fe1 N2 89.78(7) 3_565 3_565 ?
N2 Fe1 N2 92.99(8) . 3_565 ?
N2 Fe1 N2 92.98(8) 2_665 3_565 ?
O1 Fe2 Br1 110.331(14) . . ?
O1 Fe2 Br1 110.333(14) . 3_665 ?
Br1 Fe2 Br1 108.596(15) . 3_665 ?
O1 Fe2 Br1 110.333(14) . 2_655 ?
Br1 Fe2 Br1 108.597(15) . 2_655 ?
Br1 Fe2 Br1 108.596(15) 3_665 2_655 ?
O2 Fe3 Br2 110.223(15) . . ?
O2 Fe3 Br2 110.223(15) . 3_675 ?
Br2 Fe3 Br2 108.708(15) . 3_675 ?
O2 Fe3 Br2 110.223(15) . 2_765 ?
Br2 Fe3 Br2 108.710(15) . 2_765 ?
Br2 Fe3 Br2 108.710(15) 3_675 2_765 ?
Fe2 O1 Fe2 180.0 . 16_655 ?
Fe3 O2 Fe3 180.0 . 10_776 ?
C3 N2 Fe1 170.60(19) . . ?
C1 N1 Fe1 176.26(19) . . ?
N1 C1 C2 179.4(3) . . ?
N2 C3 C4 179.7(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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
Br1 Fe2 2.3634(3) . ?
Br2 Fe3 2.3566(3) . ?
Fe1 N1 2.159(2) . ?
Fe1 N1 2.159(2) 2_665 ?
Fe1 N1 2.159(2) 3_565 ?
Fe1 N2 2.163(2) . ?
Fe1 N2 2.163(2) 2_665 ?
Fe1 N2 2.163(2) 3_565 ?
Fe2 O1 1.7664(6) . ?
Fe3 O2 1.7625(6) . ?
N2 C3 1.136(3) . ?
N1 C1 1.140(3) . ?
C1 C2 1.455(3) . ?
C3 C4 1.461(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
