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#$Date: 2021-07-05 20:43:40 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707351.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_7707351
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 Co N6, 2(C2 H3 Br3 Co N), 2(C2 H3 N) 
;
_chemical_formula_sum            'C20 H30 Br6 Co3 N10'
_chemical_formula_weight         1066.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 108.941(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.34720(10)
_cell_length_b                   18.8457(3)
_cell_length_c                   12.5811(2)
_cell_measurement_reflns_used    26109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1460
_cell_measurement_theta_min      2.001
_cell_volume                     1871.96(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and 
an AFC12 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    7.743
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_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            'clear intense blue'
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       block
_exptl_crystal_F_000             1022
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0166
_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)+(0.0112P)²+1.5992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             4301
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           FeROP9
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_original_cell_volume        1871.95(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707351
_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   0.286
_shelx_estimated_absorpt_t_max   0.497
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Co1 Co 0.500000 0.500000 0.500000 0.01103(6) Uani 1 2 d S . P . .
N1 N 0.73427(18) 0.45114(8) 0.51985(12) 0.0149(3) Uani 1 1 d . . . . .
C1 C 0.8646(2) 0.42841(9) 0.53134(13) 0.0139(3) Uani 1 1 d . . . . .
C2 C 1.0310(2) 0.39960(10) 0.54424(16) 0.0205(4) Uani 1 1 d . . . . .
H2A H 1.051206 0.401029 0.471767 0.031 Uiso 1 1 calc R U . . .
H2B H 1.036816 0.350378 0.570363 0.031 Uiso 1 1 calc R U . . .
H2C H 1.117384 0.427914 0.599304 0.031 Uiso 1 1 calc R U . . .
N2 N 0.63258(18) 0.58530(8) 0.59799(12) 0.0160(3) Uani 1 1 d . . . . .
C3 C 0.7103(2) 0.62853(9) 0.65404(14) 0.0147(3) Uani 1 1 d . . . . .
C4 C 0.8089(2) 0.68489(10) 0.72400(15) 0.0208(4) Uani 1 1 d . . . . .
H4A H 0.869871 0.711176 0.681841 0.031 Uiso 1 1 calc R U . . .
H4B H 0.890456 0.664302 0.791552 0.031 Uiso 1 1 calc R U . . .
H4C H 0.733048 0.717214 0.745788 0.031 Uiso 1 1 calc R U . . .
N3 N 0.51586(18) 0.55234(8) 0.35529(12) 0.0166(3) Uani 1 1 d . . . . .
C5 C 0.5376(2) 0.57852(10) 0.28006(15) 0.0186(3) Uani 1 1 d . . . . .
C6 C 0.5683(3) 0.61188(13) 0.18427(17) 0.0331(5) Uani 1 1 d . . . . .
H6A H 0.667168 0.643113 0.210768 0.050 Uiso 1 1 calc R U . . .
H6B H 0.468844 0.639806 0.142248 0.050 Uiso 1 1 calc R U . . .
H6C H 0.589469 0.575214 0.135230 0.050 Uiso 1 1 calc R U . . .
N5 N 0.9049(2) 0.33711(9) 0.75625(14) 0.0310(4) Uani 1 1 d . . . . .
C9 C 0.9092(2) 0.37734(10) 0.82411(15) 0.0204(4) Uani 1 1 d . . . . .
C10 C 0.9156(3) 0.42842(10) 0.91234(16) 0.0244(4) Uani 1 1 d . . . . .
H10A H 0.877268 0.405653 0.969869 0.037 Uiso 1 1 calc R U . . .
H10B H 0.841597 0.468718 0.879999 0.037 Uiso 1 1 calc R U . . .
H10C H 1.032125 0.445242 0.946479 0.037 Uiso 1 1 calc R U . . .
Co2 Co 0.66787(3) 0.36648(2) 0.17430(2) 0.01333(5) Uani 1 1 d . . . . .
Br1 Br 0.87851(2) 0.45617(2) 0.23492(2) 0.01885(4) Uani 1 1 d . . . . .
Br2 Br 0.39179(2) 0.41548(2) 0.09622(2) 0.01967(4) Uani 1 1 d . . . . .
Br3 Br 0.73768(2) 0.27786(2) 0.05925(2) 0.01941(4) Uani 1 1 d . . . . .
N4 N 0.67227(19) 0.31372(8) 0.31513(12) 0.0179(3) Uani 1 1 d . . . . .
C7 C 0.6694(2) 0.28824(9) 0.39590(15) 0.0172(3) Uani 1 1 d . . . . .
C8 C 0.6655(3) 0.25673(10) 0.50050(15) 0.0235(4) Uani 1 1 d . . . . .
H8A H 0.719825 0.288908 0.563015 0.035 Uiso 1 1 calc R U . . .
H8B H 0.726418 0.211422 0.512558 0.035 Uiso 1 1 calc R U . . .
H8C H 0.547712 0.248608 0.496448 0.035 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 0.0033 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 Co1 N1 180.00(4) . 3_666 ?
N1 Co1 N2 88.45(5) . . ?
N1 Co1 N2 91.55(5) 3_666 . ?
N1 Co1 N2 91.55(5) . 3_666 ?
N1 Co1 N2 88.45(5) 3_666 3_666 ?
N2 Co1 N2 180.0 . 3_666 ?
N1 Co1 N3 90.53(5) . 3_666 ?
N1 Co1 N3 89.47(5) 3_666 3_666 ?
N2 Co1 N3 91.14(6) . 3_666 ?
N2 Co1 N3 88.86(6) 3_666 3_666 ?
N1 Co1 N3 89.47(5) . . ?
N1 Co1 N3 90.53(5) 3_666 . ?
N2 Co1 N3 88.86(6) . . ?
N2 Co1 N3 91.14(6) 3_666 . ?
N3 Co1 N3 180.0 3_666 . ?
C1 N1 Co1 176.20(14) . . ?
N1 C1 C2 179.11(19) . . ?
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 N2 Co1 176.19(14) . . ?
N2 C3 C4 178.86(19) . . ?
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 . . ?
C5 N3 Co1 174.40(14) . . ?
N3 C5 C6 179.1(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C9 C10 179.3(2) . . ?
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 . . ?
N4 Co2 Br2 107.00(4) . . ?
N4 Co2 Br1 105.50(4) . . ?
Br2 Co2 Br1 111.883(11) . . ?
N4 Co2 Br3 104.31(4) . . ?
Br2 Co2 Br3 114.391(11) . . ?
Br1 Co2 Br3 112.862(11) . . ?
C7 N4 Co2 175.15(15) . . ?
N4 C7 C8 179.00(19) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
Co1 N1 2.1017(14) . ?
Co1 N1 2.1017(14) 3_666 ?
Co1 N2 2.1079(15) . ?
Co1 N2 2.1079(15) 3_666 ?
Co1 N3 2.1122(15) 3_666 ?
Co1 N3 2.1122(15) . ?
N1 C1 1.134(2) . ?
C1 C2 1.450(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 C3 1.134(2) . ?
C3 C4 1.453(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N3 C5 1.133(2) . ?
C5 C6 1.454(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N5 C9 1.134(3) . ?
C9 C10 1.457(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Co2 N4 2.0216(15) . ?
Co2 Br2 2.3789(3) . ?
Co2 Br1 2.3789(3) . ?
Co2 Br3 2.4025(3) . ?
N4 C7 1.131(2) . ?
C7 C8 1.454(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
