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#$Date: 2021-03-05 04:10:13 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262662 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/57/7705775.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_7705775
loop_
_publ_author_name
'Plajer, Alex J.'
'Crusius, Daniel'
'Jethwa, Rajesh B.'
'García-Romero, Álvaro'
'Bond, Andrew D.'
'García-Rodríguez, Raúl'
'Wright, Dominic S.'
_publ_section_title
;
 Coordination chemistry of the bench-stable tris-2-pyridyl pnictogen
 ligands [E(6-Me-2-py)₃] (E = As, As[double bond, length as
 m-dash]O, Sb).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2393
_journal_page_last               2402
_journal_paper_doi               10.1039/d0dt03732j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H18 As Br2 Co N3'
_chemical_formula_sum            'C18 H18 As Br2 Co N3'
_chemical_formula_weight         570.02
_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-2018/1
_audit_update_record
;
2020-10-20 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                101.1675(15)
_cell_angle_beta                 93.4356(14)
_cell_angle_gamma                115.3045(13)
_cell_formula_units_Z            2
_cell_length_a                   8.2686(2)
_cell_length_b                   8.6144(3)
_cell_length_c                   15.8017(5)
_cell_measurement_reflns_used    7300
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.57
_cell_measurement_theta_min      2.89
_cell_volume                     985.27(5)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12450
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.580
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_min         2.888
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    13.486
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       block
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0265
_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)+(0.0325P)²+0.0821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3048
_reflns_number_total             3447
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03732j2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7705770--7705782.cif.'
_cod_database_code               7705775
_cambridge_user_name             'Alex Plajer'
_cambridge_user_crsid            ajp233
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             DC_CoCl2As(III)
_cambridge_data_id               DW_B1_0284
_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   0.294
_shelx_estimated_absorpt_t_max   0.377
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
As1 As 0.72221(4) 0.58700(4) 0.21320(2) 0.02061(10) Uani 1 1 d . . . . .
Br1 Br 0.02203(4) 0.20009(4) 0.09151(2) 0.02544(10) Uani 1 1 d . . . . .
Br2 Br 0.16649(5) 0.55468(5) 0.33352(2) 0.03364(11) Uani 1 1 d . . . . .
Co1 Co 0.25035(6) 0.42448(6) 0.20855(3) 0.01707(12) Uani 1 1 d . . . . .
N1 N 0.7281(4) 0.8653(4) 0.34161(17) 0.0270(6) Uani 1 1 d . . . . .
N2 N 0.3941(3) 0.2909(3) 0.23511(16) 0.0194(5) Uani 1 1 d . . . . .
N3 N 0.3968(3) 0.6110(3) 0.14402(15) 0.0157(5) Uani 1 1 d . . . . .
C1 C 0.6989(4) 0.6973(4) 0.3299(2) 0.0241(7) Uani 1 1 d . . . . .
C2 C 0.6825(6) 0.6130(5) 0.3978(3) 0.0486(11) Uani 1 1 d . . . . .
H2A H 0.666077 0.494419 0.387449 0.058 Uiso 1 1 calc R U . . .
C3 C 0.6907(7) 0.7070(6) 0.4808(3) 0.0657(15) Uani 1 1 d . . . . .
H3A H 0.678748 0.653458 0.528741 0.079 Uiso 1 1 calc R U . . .
C4 C 0.7161(6) 0.8765(6) 0.4930(3) 0.0578(13) Uani 1 1 d . . . . .
H4A H 0.718955 0.941104 0.549510 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7379(5) 0.9561(5) 0.4234(2) 0.0375(9) Uani 1 1 d . . . . .
C6 C 0.7795(7) 1.1476(6) 0.4358(3) 0.0600(13) Uani 1 1 d . . . . .
H6A H 0.839319 1.192425 0.387959 0.090 Uiso 1 1 calc R U . . .
H6B H 0.859885 1.216207 0.491625 0.090 Uiso 1 1 calc R U . . .
H6C H 0.666585 1.158961 0.435965 0.090 Uiso 1 1 calc R U . . .
C7 C 0.5650(4) 0.3426(4) 0.2167(2) 0.0205(7) Uani 1 1 d . . . . .
C8 C 0.6515(5) 0.2360(4) 0.2133(2) 0.0273(7) Uani 1 1 d . . . . .
H8A H 0.768680 0.273443 0.197077 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5651(5) 0.0735(4) 0.2338(2) 0.0321(8) Uani 1 1 d . . . . .
H9A H 0.621386 -0.002741 0.231401 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3972(5) 0.0254(4) 0.2575(2) 0.0322(8) Uani 1 1 d . . . . .
H10A H 0.339182 -0.082239 0.275020 0.039 Uiso 1 1 calc R U . . .
C11 C 0.3103(4) 0.1323(4) 0.2561(2) 0.0246(7) Uani 1 1 d . . . . .
C12 C 0.1244(5) 0.0768(5) 0.2787(2) 0.0343(8) Uani 1 1 d . . . . .
H12A H 0.117757 0.178616 0.315697 0.051 Uiso 1 1 calc R U . . .
H12B H 0.096981 -0.016665 0.310144 0.051 Uiso 1 1 calc R U . . .
H12C H 0.036102 0.032048 0.224925 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5721(4) 0.6460(4) 0.13701(19) 0.0170(6) Uani 1 1 d . . . . .
C14 C 0.6599(4) 0.7331(4) 0.0767(2) 0.0221(7) Uani 1 1 d . . . . .
H14A H 0.781903 0.755773 0.073102 0.026 Uiso 1 1 calc R U . . .
C15 C 0.5693(4) 0.7881(4) 0.0208(2) 0.0253(7) Uani 1 1 d . . . . .
H15A H 0.626492 0.844280 -0.022697 0.030 Uiso 1 1 calc R U . . .
C16 C 0.3956(4) 0.7588(4) 0.0305(2) 0.0246(7) Uani 1 1 d . . . . .
H16A H 0.331990 0.797376 -0.005767 0.029 Uiso 1 1 calc R U . . .
C17 C 0.3121(4) 0.6725(4) 0.09344(19) 0.0185(6) Uani 1 1 d . . . . .
C18 C 0.1262(4) 0.6487(4) 0.1072(2) 0.0241(7) Uani 1 1 d . . . . .
H18A H 0.119513 0.666618 0.169805 0.036 Uiso 1 1 calc R U . . .
H18B H 0.036637 0.528802 0.076425 0.036 Uiso 1 1 calc R U . . .
H18C H 0.100633 0.735297 0.084347 0.036 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'
As As -0.9300 1.0051 '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'
Co Co -2.3653 3.6143 '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
C7 As1 C13 104.22(12) . . ?
C7 As1 C1 96.09(13) . . ?
C13 As1 C1 101.83(12) . . ?
N3 Co1 N2 109.07(10) . . ?
N3 Co1 Br2 110.91(7) . . ?
N2 Co1 Br2 113.93(7) . . ?
N3 Co1 Br1 101.64(7) . . ?
N2 Co1 Br1 99.52(7) . . ?
Br2 Co1 Br1 120.46(2) . . ?
C1 N1 C5 118.0(3) . . ?
C7 N2 C11 118.2(3) . . ?
C7 N2 Co1 120.1(2) . . ?
C11 N2 Co1 120.6(2) . . ?
C17 N3 C13 118.6(2) . . ?
C17 N3 Co1 120.20(19) . . ?
C13 N3 Co1 119.79(19) . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 As1 115.1(2) . . ?
C2 C1 As1 120.8(3) . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 H2A 121.0 . . ?
C1 C2 H2A 121.0 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3A 120.4 . . ?
C2 C3 H3A 120.4 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 117.1(3) . . ?
C4 C5 C6 121.7(4) . . ?
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 . . ?
N2 C7 C8 122.5(3) . . ?
N2 C7 As1 122.3(2) . . ?
C8 C7 As1 114.4(2) . . ?
C7 C8 C9 119.1(3) . . ?
C7 C8 H8A 120.4 . . ?
C9 C8 H8A 120.4 . . ?
C10 C9 C8 118.5(3) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 H10A 119.6 . . ?
C11 C10 H10A 119.6 . . ?
N2 C11 C10 120.7(3) . . ?
N2 C11 C12 118.5(3) . . ?
C10 C11 C12 120.8(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 121.6(3) . . ?
N3 C13 As1 123.8(2) . . ?
C14 C13 As1 114.5(2) . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 118.2(3) . . ?
C16 C15 H15A 120.9 . . ?
C14 C15 H15A 120.9 . . ?
C15 C16 C17 120.2(3) . . ?
C15 C16 H16A 119.9 . . ?
C17 C16 H16A 119.9 . . ?
N3 C17 C16 121.3(3) . . ?
N3 C17 C18 118.5(3) . . ?
C16 C17 C18 120.2(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
As1 C7 1.959(3) . ?
As1 C13 1.961(3) . ?
As1 C1 1.965(3) . ?
Br1 Co1 2.4080(6) . ?
Br2 Co1 2.3684(6) . ?
Co1 N3 2.051(2) . ?
Co1 N2 2.052(2) . ?
N1 C1 1.334(4) . ?
N1 C5 1.353(4) . ?
N2 C7 1.358(4) . ?
N2 C11 1.360(4) . ?
N3 C17 1.350(4) . ?
N3 C13 1.365(4) . ?
C1 C2 1.389(5) . ?
C2 C3 1.383(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.355(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.385(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.503(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.380(4) . ?
C8 C9 1.387(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.368(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.391(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.491(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.375(4) . ?
C14 C15 1.397(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.371(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.396(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.497(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -1.6(5) . . . . ?
C5 N1 C1 As1 -171.4(2) . . . . ?
N1 C1 C2 C3 2.3(6) . . . . ?
As1 C1 C2 C3 171.6(3) . . . . ?
C1 C2 C3 C4 -0.7(7) . . . . ?
C2 C3 C4 C5 -1.5(8) . . . . ?
C1 N1 C5 C4 -0.7(5) . . . . ?
C1 N1 C5 C6 177.2(3) . . . . ?
C3 C4 C5 N1 2.3(7) . . . . ?
C3 C4 C5 C6 -175.5(5) . . . . ?
C11 N2 C7 C8 4.1(5) . . . . ?
Co1 N2 C7 C8 -164.2(2) . . . . ?
C11 N2 C7 As1 -164.9(2) . . . . ?
Co1 N2 C7 As1 26.8(3) . . . . ?
N2 C7 C8 C9 -3.4(5) . . . . ?
As1 C7 C8 C9 166.4(3) . . . . ?
C7 C8 C9 C10 -0.6(5) . . . . ?
C8 C9 C10 C11 3.7(5) . . . . ?
C7 N2 C11 C10 -0.9(4) . . . . ?
Co1 N2 C11 C10 167.4(2) . . . . ?
C7 N2 C11 C12 178.5(3) . . . . ?
Co1 N2 C11 C12 -13.3(4) . . . . ?
C9 C10 C11 N2 -3.0(5) . . . . ?
C9 C10 C11 C12 177.6(3) . . . . ?
C17 N3 C13 C14 -3.6(4) . . . . ?
Co1 N3 C13 C14 162.9(2) . . . . ?
C17 N3 C13 As1 173.8(2) . . . . ?
Co1 N3 C13 As1 -19.7(3) . . . . ?
N3 C13 C14 C15 0.0(5) . . . . ?
As1 C13 C14 C15 -177.6(2) . . . . ?
C13 C14 C15 C16 2.5(5) . . . . ?
C14 C15 C16 C17 -1.5(5) . . . . ?
C13 N3 C17 C16 4.7(4) . . . . ?
Co1 N3 C17 C16 -161.8(2) . . . . ?
C13 N3 C17 C18 -174.3(3) . . . . ?
Co1 N3 C17 C18 19.2(4) . . . . ?
C15 C16 C17 N3 -2.2(5) . . . . ?
C15 C16 C17 C18 176.8(3) . . . . ?
