#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:09:13 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258819 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705494.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_7705494
loop_
_publ_author_name
'Kirkman-Davis, Emma'
'Witkos, Faith E.'
'Selmani, Veli'
'Monroe, Jeffrey C.'
'Landee, Christopher P.'
'Turnbull, Mark M.'
'Dawe, Louise N.'
'Polson, Matthew I. J.'
'Wikaira, Jan L.'
_publ_section_title
;
 Pyrazine-bridged Cu(ii) chains: diaquabis(n-methyl-2-pyridone)copper(ii)
 perchlorate complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13693
_journal_page_last               13703
_journal_paper_doi               10.1039/d0dt02716b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C16 H22 Cl2 Cu N4 O12'
_chemical_formula_weight         596.81
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2020-09-10 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.864(15)
_cell_angle_beta                 99.515(17)
_cell_angle_gamma                93.963(16)
_cell_formula_units_Z            1
_cell_length_a                   6.8276(15)
_cell_length_b                   8.1623(12)
_cell_length_c                   10.464(2)
_cell_measurement_reflns_used    1876
_cell_measurement_temperature    280.00(10)
_cell_measurement_theta_max      28.8270
_cell_measurement_theta_min      3.8440
_cell_volume                     573.54(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      280.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4052
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            blue-green
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       prism
_exptl_crystal_F_000             305
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0640
_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)+(0.1194P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2869
_reflns_number_total             4052
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02716b2.cif
_cod_data_source_block           ekdoa
_cod_depositor_comments
'Adding full bibliography for 7705494--7705499.cif.'
_cod_original_cell_volume        573.55(19)
_cod_database_code               7705494
_shelx_shelxl_version_number     2016/4
_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.
;
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
CU1 Cu -0.500000 0.500000 0.500000 0.0338(3) Uani 1 2 d S . P . .
N1 N -0.2014(5) 0.4988(4) 0.4995(3) 0.0260(7) Uani 1 1 d . . . . .
C2 C -0.0912(6) 0.3904(5) 0.5682(4) 0.0329(10) Uani 1 1 d . . . . .
H2 H -0.151618 0.313081 0.616320 0.040 Uiso 1 1 calc R U . . .
C3 C -0.1096(6) 0.6075(5) 0.4318(4) 0.0322(10) Uani 1 1 d . . . . .
H3 H -0.183409 0.683754 0.383497 0.039 Uiso 1 1 calc R U . . .
N11 N -0.3469(6) 0.6480(5) 0.8075(4) 0.0457(10) Uani 1 1 d . . . . .
H11 H -0.389(8) 0.704(7) 0.746(6) 0.055 Uiso 1 1 d . U . . .
C12 C -0.3802(6) 0.4836(5) 0.7881(4) 0.0337(10) Uani 1 1 d . . . . .
O12 O -0.4622(5) 0.4237(4) 0.6762(3) 0.0368(7) Uani 1 1 d . . . . .
C13 C -0.3204(7) 0.3834(6) 0.8948(4) 0.0362(10) Uani 1 1 d . . . . .
C14 C -0.2418(7) 0.4598(7) 1.0115(5) 0.0471(12) Uani 1 1 d . . . . .
H14 H -0.205270 0.395782 1.083122 0.057 Uiso 1 1 calc R U . . .
C15 C -0.2151(8) 0.6294(7) 1.0261(5) 0.0542(14) Uani 1 1 d . . . . .
H15 H -0.162658 0.677941 1.106543 0.065 Uiso 1 1 calc R U . . .
C16 C -0.2651(8) 0.7220(7) 0.9242(6) 0.0542(14) Uani 1 1 d . . . . .
H16 H -0.244759 0.835763 0.932074 0.065 Uiso 1 1 calc R U . . .
C17 C -0.3489(9) 0.2019(7) 0.8750(5) 0.0535(13) Uani 1 1 d . . . . .
H17A H -0.259548 0.166489 0.820100 0.064 Uiso 1 1 calc R U . . .
H17B H -0.483747 0.171900 0.835017 0.064 Uiso 1 1 calc R U . . .
H17C H -0.321716 0.150291 0.957279 0.064 Uiso 1 1 calc R U . . .
O1W O -0.4536(6) 0.7975(5) 0.5666(4) 0.0515(9) Uani 1 1 d D . . . .
H1WA H -0.544(7) 0.856(6) 0.579(5) 0.062 Uiso 1 1 d D U . . .
H1WB H -0.366(7) 0.862(6) 0.548(5) 0.062 Uiso 1 1 d D U . . .
CL1 Cl 0.1217(2) 0.93269(15) 0.70919(13) 0.0540(4) Uani 1 1 d . . . . .
O1 O -0.008(3) 0.807(2) 0.6718(19) 0.099(7) Uani 0.434(12) 1 d . . P A 1
O2 O 0.2940(19) 0.878(2) 0.7943(12) 0.107(6) Uani 0.434(12) 1 d . . P A 1
O3 O 0.065(3) 1.0733(14) 0.7428(16) 0.111(7) Uani 0.434(12) 1 d . . P A 1
O4 O 0.262(3) 1.007(2) 0.6491(18) 0.065(4) Uani 0.434(12) 1 d . . P A 1
O1' O 0.095(3) 0.7601(15) 0.7103(15) 0.092(5) Uani 0.566(12) 1 d . . P A 2
O2' O 0.1487(19) 0.9921(14) 0.8425(9) 0.107(5) Uani 0.566(12) 1 d . . P A 2
O3' O -0.0826(13) 0.9861(15) 0.6601(11) 0.098(4) Uani 0.566(12) 1 d . . P A 2
O4' O 0.221(2) 0.9683(19) 0.5928(14) 0.068(3) Uani 0.566(12) 1 d . . P A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O12 CU1 O12 180.00(18) 2_466 . ?
O12 CU1 N1 89.86(13) 2_466 . ?
O12 CU1 N1 90.14(13) . . ?
O12 CU1 N1 90.14(13) 2_466 2_466 ?
O12 CU1 N1 89.86(13) . 2_466 ?
N1 CU1 N1 180.0 . 2_466 ?
C3 N1 C2 117.9(3) . . ?
C3 N1 CU1 120.7(3) . . ?
C2 N1 CU1 121.4(3) . . ?
N1 C2 C3 120.7(4) . 2_566 ?
N1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 2_566 . ?
N1 C3 C2 121.4(4) . 2_566 ?
N1 C3 H3 119.3 . . ?
C2 C3 H3 119.3 2_566 . ?
C12 N11 C16 123.9(5) . . ?
C12 N11 H11 116(4) . . ?
C16 N11 H11 120(4) . . ?
O12 C12 N11 120.1(4) . . ?
O12 C12 C13 122.5(4) . . ?
N11 C12 C13 117.3(4) . . ?
C12 O12 CU1 136.0(3) . . ?
C14 C13 C12 117.9(4) . . ?
C14 C13 C17 123.6(5) . . ?
C12 C13 C17 118.5(4) . . ?
C13 C14 C15 122.1(5) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 N11 119.3(5) . . ?
C15 C16 H16 120.4 . . ?
N11 C16 H16 120.4 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H1WA O1W H1WB 105(6) . . ?
O3a CL1 O1 121.4(13) . . ?
O3a CL1 O4 91.4(11) . . ?
O1a CL1 O4 130.6(11) . . ?
O1'b CL1 O2' 107.2(8) . . ?
O3a CL1 O2 114.5(11) . . ?
O1a CL1 O2 110.2(12) . . ?
O4a CL1 O2 82.9(10) . . ?
O1'b CL1 O3' 104.2(8) . . ?
O2'b CL1 O3' 100.3(7) . . ?
O1'b CL1 O4' 104.7(9) . . ?
O2'b CL1 O4' 136.0(8) . . ?
O3'b CL1 O4' 100.2(7) . . ?
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
CU1 O12 1.937(3) 2_466 ?
CU1 O12 1.937(3) . ?
CU1 N1 2.040(3) . ?
CU1 N1 2.040(3) 2_466 ?
N1 C3 1.331(5) . ?
N1 C2 1.341(5) . ?
C2 C3 1.370(5) 2_566 ?
C2 H2 0.9300 . ?
C3 C2 1.370(5) 2_566 ?
C3 H3 0.9300 . ?
N11 C12 1.352(6) . ?
N11 C16 1.369(7) . ?
N11 H11 0.82(6) . ?
C12 O12 1.285(5) . ?
C12 C13 1.415(6) . ?
C13 C14 1.372(7) . ?
C13 C17 1.488(7) . ?
C14 C15 1.386(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.328(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O1W H1WA 0.83(3) . ?
O1W H1WB 0.82(3) . ?
CL1 O3 1.297(10) . ?
CL1 O1 1.317(14) . ?
CL1 O4 1.34(2) . ?
CL1 O1' 1.408(13) . ?
CL1 O2' 1.449(9) . ?
CL1 O2 1.454(11) . ?
CL1 O3' 1.501(9) . ?
CL1 O4' 1.512(16) . ?
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
C3 N1 C2 C3 0.0(6) . . . 2_566 ?
CU1 N1 C2 C3 -179.2(3) . . . 2_566 ?
C2 N1 C3 C2 0.0(6) . . . 2_566 ?
CU1 N1 C3 C2 179.2(3) . . . 2_566 ?
C16 N11 C12 O12 178.3(4) . . . . ?
C16 N11 C12 C13 -2.0(7) . . . . ?
N11 C12 O12 CU1 20.1(6) . . . . ?
C13 C12 O12 CU1 -159.6(3) . . . . ?
O12 C12 C13 C14 -177.3(4) . . . . ?
N11 C12 C13 C14 3.0(6) . . . . ?
O12 C12 C13 C17 1.7(7) . . . . ?
N11 C12 C13 C17 -177.9(4) . . . . ?
C12 C13 C14 C15 -1.8(7) . . . . ?
C17 C13 C14 C15 179.2(5) . . . . ?
C13 C14 C15 C16 -0.6(8) . . . . ?
C14 C15 C16 N11 1.7(8) . . . . ?
C12 N11 C16 C15 -0.4(8) . . . . ?
