#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:10:13 +0100 (vie 05 de mar de 2021) $
#$Revision: 262662 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/57/7705770.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_7705770
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         'C20 H21 As Cu N4 O +, F6 P -'
_chemical_formula_sum            'C20 H21 As Cu F6 N4 O P'
_chemical_formula_weight         616.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8006(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9397(5)
_cell_length_b                   14.5346(4)
_cell_length_c                   8.8190(2)
_cell_measurement_reflns_used    4908
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.58
_cell_measurement_theta_min      3.91
_cell_volume                     2298.39(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7344
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.578
_diffrn_reflns_theta_max         66.578
_diffrn_reflns_theta_min         3.915
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    4.253
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00042(4)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2110
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0261
_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)+(0.0288P)²+3.6258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1887
_reflns_number_total             2110
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03732j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7705770--7705782.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7705770
_cambridge_user_name             'Alex Plajer'
_cambridge_user_crsid            ajp33
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             DS_As(V)CuPF6
_cambridge_data_id               DW_B1_0290
_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   0.455
_shelx_estimated_absorpt_t_max   0.784
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.16354(2) 0.500000 0.40470(4) 0.01913(13) Uani 1 2 d S T P . .
Cu1 Cu 0.31858(2) 0.500000 0.57197(5) 0.02420(15) Uani 1 2 d S T P . .
O1 O 0.08242(12) 0.500000 0.3151(3) 0.0293(6) Uani 1 2 d S T P . .
N1 N 0.22389(14) 0.500000 0.7025(3) 0.0188(6) Uani 1 2 d S T P . .
N2 N 0.29050(9) 0.61304(14) 0.4264(2) 0.0203(4) Uani 1 1 d . . . . .
N3 N 0.41938(15) 0.500000 0.6610(3) 0.0277(7) Uani 1 2 d S T P . .
C1 C 0.15851(16) 0.500000 0.6229(3) 0.0192(7) Uani 1 2 d S T P . .
C2 C 0.08897(17) 0.500000 0.6855(4) 0.0253(7) Uani 1 2 d S T P . .
H2A H 0.044647 0.500000 0.623618 0.030 Uiso 1 2 calc R U P . .
C3 C 0.08657(19) 0.500000 0.8425(4) 0.0306(8) Uani 1 2 d S T P . .
H3A H 0.040082 0.500000 0.891176 0.037 Uiso 1 2 calc R U P . .
C4 C 0.1523(2) 0.500000 0.9267(4) 0.0303(8) Uani 1 2 d S T P . .
H4A H 0.151225 0.500000 1.034356 0.036 Uiso 1 2 calc R U P . .
C5 C 0.22074(18) 0.500000 0.8555(4) 0.0222(7) Uani 1 2 d S T P . .
C6 C 0.2931(2) 0.500000 0.9456(4) 0.0315(8) Uani 1 2 d S T P . .
H6A H 0.285499 0.500000 1.055168 0.047 Uiso 1 2 d R U P . .
H6B H 0.321039 0.554210 0.913498 0.047 Uiso 1 1 d R U . . .
C7 C 0.22297(12) 0.60563(17) 0.3553(2) 0.0208(5) Uani 1 1 d . . . . .
C8 C 0.19356(13) 0.66803(19) 0.2520(3) 0.0272(5) Uani 1 1 d . . . . .
H8A H 0.145352 0.659702 0.206365 0.033 Uiso 1 1 calc R U . . .
C9 C 0.23724(16) 0.74349(19) 0.2173(3) 0.0347(6) Uani 1 1 d . . . . .
H9A H 0.219938 0.787655 0.145007 0.042 Uiso 1 1 calc R U . . .
C10 C 0.30599(15) 0.75343(19) 0.2892(3) 0.0315(6) Uani 1 1 d . . . . .
H10A H 0.336321 0.804941 0.266727 0.038 Uiso 1 1 calc R U . . .
C11 C 0.33133(12) 0.68833(18) 0.3947(3) 0.0253(5) Uani 1 1 d . . . . .
C12 C 0.40518(13) 0.6999(2) 0.4758(3) 0.0348(6) Uani 1 1 d . . . . .
H12A H 0.400221 0.685282 0.583524 0.052 Uiso 1 1 calc R U . . .
H12B H 0.422070 0.763634 0.465419 0.052 Uiso 1 1 calc R U . . .
H12C H 0.441648 0.658327 0.431702 0.052 Uiso 1 1 calc R U . . .
C13 C 0.47778(19) 0.500000 0.7124(4) 0.0256(7) Uani 1 2 d S T P . .
C14 C 0.55366(19) 0.500000 0.7768(5) 0.0348(9) Uani 1 2 d S T P . .
H14A H 0.589792 0.500000 0.695716 0.052 Uiso 1 2 d R U P . .
H14B H 0.561812 0.554850 0.839785 0.052 Uiso 1 1 d R U . . .
P1 P 0.500000 0.74064(7) 1.000000 0.0308(2) Uani 1 2 d DS T P . .
F1 F 0.5005(3) 0.7114(3) 1.1715(5) 0.0752(18) Uani 0.5 1 d D . P A -1
F2 F 0.4579(2) 0.6478(3) 0.9541(5) 0.0704(13) Uani 0.5 1 d D . P A -1
F3 F 0.4208(2) 0.7881(4) 1.0181(5) 0.0662(13) Uani 0.5 1 d D . P A -1
F4 F 0.5779(2) 0.6926(4) 0.9812(6) 0.0818(16) Uani 0.5 1 d D . P A -1
F5 F 0.5395(2) 0.8336(3) 1.0413(5) 0.0714(13) Uani 0.5 1 d D . P A -1
F6 F 0.4969(3) 0.7679(4) 0.8253(5) 0.0740(17) Uani 0.5 1 d D . P 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 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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'
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
O1 As1 C7 112.41(8) . . ?
O1 As1 C7 112.41(8) . 6_565 ?
C7 As1 C7 105.65(13) . 6_565 ?
O1 As1 C1 114.43(12) . . ?
C7 As1 C1 105.62(8) . . ?
C7 As1 C1 105.62(8) 6_565 . ?
N3 Cu1 N1 122.71(11) . . ?
N3 Cu1 N2 116.14(7) . 6_565 ?
N1 Cu1 N2 98.70(7) . 6_565 ?
N3 Cu1 N2 116.14(7) . . ?
N1 Cu1 N2 98.70(7) . . ?
N2 Cu1 N2 100.58(10) 6_565 . ?
C1 N1 C5 117.2(3) . . ?
C1 N1 Cu1 115.1(2) . . ?
C5 N1 Cu1 127.8(2) . . ?
C7 N2 C11 116.9(2) . . ?
C7 N2 Cu1 114.14(16) . . ?
C11 N2 Cu1 128.93(15) . . ?
C13 N3 Cu1 179.9(3) . . ?
N1 C1 C2 125.1(3) . . ?
N1 C1 As1 116.9(2) . . ?
C2 C1 As1 118.0(2) . . ?
C1 C2 C3 117.1(3) . . ?
C1 C2 H2A 121.4 . . ?
C3 C2 H2A 121.4 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3A 120.4 . . ?
C2 C3 H3A 120.4 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
N1 C5 C4 120.9(3) . . ?
N1 C5 C6 117.7(3) . . ?
C4 C5 C6 121.4(3) . . ?
C5 C6 H6A 112.1 . . ?
C5 C6 H6B 106.8 . . ?
H6A C6 H6B 111.9 . . ?
C5 C6 H6B 106.76(10) . 6_565 ?
H6A C6 H6B 111.9 . 6_565 ?
H6B C6 H6B 107.0 . 6_565 ?
N2 C7 C8 125.0(2) . . ?
N2 C7 As1 116.94(17) . . ?
C8 C7 As1 118.08(17) . . ?
C7 C8 C9 117.3(2) . . ?
C7 C8 H8A 121.4 . . ?
C9 C8 H8A 121.4 . . ?
C10 C9 C8 119.0(2) . . ?
C10 C9 H9A 120.5 . . ?
C8 C9 H9A 120.5 . . ?
C9 C10 C11 120.3(2) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
N2 C11 C10 121.4(2) . . ?
N2 C11 C12 118.0(2) . . ?
C10 C11 C12 120.6(2) . . ?
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 179.2(4) . . ?
C13 C14 H14A 110.3 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.9 . . ?
C13 C14 H14B 109.97(11) . 6_565 ?
H14A C14 H14B 108.9 . 6_565 ?
H14B C14 H14B 108.9 . 6_565 ?
F5 P1 F1 91.2(2) . . ?
F5 P1 F4 90.6(2) . . ?
F1 P1 F4 90.1(3) . . ?
F5 P1 F6 90.7(3) . . ?
F1 P1 F6 177.9(3) . . ?
F4 P1 F6 90.7(3) . . ?
F5 P1 F3 90.1(3) . . ?
F1 P1 F3 89.9(3) . . ?
F4 P1 F3 179.3(3) . . ?
F6 P1 F3 89.2(2) . . ?
F5 P1 F2 178.1(2) . . ?
F1 P1 F2 90.2(3) . . ?
F4 P1 F2 90.7(3) . . ?
F6 P1 F2 87.9(2) . . ?
F3 P1 F2 88.6(2) . . ?
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 O1 1.634(2) . ?
As1 C7 1.927(2) . ?
As1 C7 1.927(2) 6_565 ?
As1 C1 1.929(3) . ?
Cu1 N3 1.948(3) . ?
Cu1 N1 2.082(3) . ?
Cu1 N2 2.136(2) 6_565 ?
Cu1 N2 2.136(2) . ?
N1 C1 1.348(4) . ?
N1 C5 1.353(4) . ?
N2 C7 1.351(3) . ?
N2 C11 1.351(3) . ?
N3 C13 1.128(4) . ?
C1 C2 1.380(4) . ?
C2 C3 1.387(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.374(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.396(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.501(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6B 0.9800 6_565 ?
C7 C8 1.379(3) . ?
C8 C9 1.388(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.377(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.393(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.495(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.459(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9801 . ?
C14 H14B 0.9800 6_565 ?
P1 F5 1.563(4) . ?
P1 F1 1.571(4) . ?
P1 F4 1.575(4) . ?
P1 F6 1.590(4) . ?
P1 F3 1.591(3) . ?
P1 F2 1.592(4) . ?
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 0.000(1) . . . . ?
Cu1 N1 C1 C2 180.000(1) . . . . ?
C5 N1 C1 As1 180.000(0) . . . . ?
Cu1 N1 C1 As1 0.000(1) . . . . ?
N1 C1 C2 C3 0.000(1) . . . . ?
As1 C1 C2 C3 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(1) . . . . ?
C2 C3 C4 C5 0.000(1) . . . . ?
C1 N1 C5 C4 0.000(1) . . . . ?
Cu1 N1 C5 C4 180.000(1) . . . . ?
C1 N1 C5 C6 180.000(1) . . . . ?
Cu1 N1 C5 C6 0.000(1) . . . . ?
C3 C4 C5 N1 0.000(1) . . . . ?
C3 C4 C5 C6 180.000(1) . . . . ?
C11 N2 C7 C8 1.1(3) . . . . ?
Cu1 N2 C7 C8 -177.64(19) . . . . ?
C11 N2 C7 As1 -178.31(16) . . . . ?
Cu1 N2 C7 As1 3.0(2) . . . . ?
N2 C7 C8 C9 0.9(4) . . . . ?
As1 C7 C8 C9 -179.76(19) . . . . ?
C7 C8 C9 C10 -1.5(4) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C7 N2 C11 C10 -2.4(3) . . . . ?
Cu1 N2 C11 C10 176.13(17) . . . . ?
C7 N2 C11 C12 177.9(2) . . . . ?
Cu1 N2 C11 C12 -3.6(3) . . . . ?
C9 C10 C11 N2 1.8(4) . . . . ?
C9 C10 C11 C12 -178.6(2) . . . . ?
