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#$Date: 2020-11-06 14:09:13 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258819 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705499.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_7705499
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-2018/3
_audit_update_record
;
2020-07-19 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.984(8)
_cell_angle_beta                 99.500(7)
_cell_angle_gamma                93.911(8)
_cell_formula_units_Z            1
_cell_length_a                   6.8314(6)
_cell_length_b                   8.1609(9)
_cell_length_c                   10.4545(10)
_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                     573.27(10)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHelxl-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 0.968
_diffrn_measured_fraction_theta_max 0.811
_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     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5016
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.708
_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    1.729
_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         2.708
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0792
_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)+(0.1312P)²+0.1365P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3882
_reflns_number_total             5016
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02716b2.cif
_cod_data_source_block           ekdoa_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705494--7705499.cif.'
_cod_original_cell_volume        573.28(10)
_cod_database_code               7705499
_shelx_shelxl_version_number     2018/3
_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 0.0336(3) Uani 1 2 d S . P . .
N1 N -0.1980(5) 0.4993(4) 0.4997(3) 0.0240(7) Uani 1 1 d . . . . .
C2 C -0.0925(7) 0.3907(6) 0.5672(4) 0.0329(10) Uani 1 1 d . . . . .
H2 H -0.154450 0.312990 0.614139 0.039 Uiso 1 1 calc R U . . .
C3 C -0.1100(7) 0.6075(6) 0.4321(4) 0.0329(10) Uani 1 1 d . . . . .
H3 H -0.184458 0.683042 0.383518 0.039 Uiso 1 1 calc R U . . .
N11 N -0.3465(8) 0.6478(6) 0.8076(5) 0.0470(12) Uani 1 1 d . . . . .
H11 H -0.380(11) 0.707(8) 0.746(6) 0.056 Uiso 1 1 d . U . . .
C12 C -0.3794(7) 0.4838(6) 0.7882(5) 0.0347(11) Uani 1 1 d . . . . .
O12 O -0.4621(5) 0.4240(5) 0.6769(3) 0.0376(8) Uani 1 1 d . . . . .
C13 C -0.3215(8) 0.3830(7) 0.8952(5) 0.0372(11) Uani 1 1 d . . . . .
C14 C -0.2420(9) 0.4601(8) 1.0111(5) 0.0471(14) Uani 1 1 d . . . . .
H14 H -0.204947 0.396336 1.082716 0.057 Uiso 1 1 calc R U . . .
C15 C -0.2146(10) 0.6298(9) 1.0259(6) 0.0553(16) Uani 1 1 d . . . . .
H15 H -0.161175 0.678563 1.106262 0.066 Uiso 1 1 calc R U . . .
C16 C -0.2653(10) 0.7214(8) 0.9242(6) 0.0545(16) Uani 1 1 d . . . . .
H16 H -0.245800 0.835247 0.932193 0.065 Uiso 1 1 calc R U . . .
C17 C -0.3478(11) 0.2021(8) 0.8752(6) 0.0538(15) Uani 1 1 d . . . . .
H17A H -0.256401 0.167218 0.821417 0.065 Uiso 1 1 calc R U . . .
H17B H -0.481658 0.171322 0.833688 0.065 Uiso 1 1 calc R U . . .
H17C H -0.322369 0.150549 0.957565 0.065 Uiso 1 1 calc R U . . .
O1W O -0.4546(7) 0.7976(5) 0.5661(4) 0.0527(10) Uani 1 1 d D . . . .
H1A H -0.546(8) 0.862(7) 0.569(6) 0.063 Uiso 1 1 d D U . . .
H1B H -0.349(7) 0.855(8) 0.565(6) 0.063 Uiso 1 1 d D U . . .
Cl1 Cl 0.1214(3) 0.93275(18) 0.70919(14) 0.0554(5) Uani 1 1 d . . . . .
O1 O -0.005(4) 0.806(3) 0.671(2) 0.106(9) Uani 0.449(15) 1 d . . P A 1
O2 O 0.289(3) 0.882(3) 0.7959(14) 0.120(8) Uani 0.449(15) 1 d . . P A 1
O3 O 0.068(3) 1.0745(17) 0.7441(17) 0.113(8) Uani 0.449(15) 1 d . . P A 1
O4 O 0.258(4) 1.005(3) 0.645(2) 0.069(5) Uani 0.449(15) 1 d . . P A 1
O1' O 0.094(3) 0.7604(19) 0.7117(18) 0.092(6) Uani 0.551(15) 1 d . . P A 2
O2' O 0.146(2) 0.9932(17) 0.8430(11) 0.105(6) Uani 0.551(15) 1 d . . P A 2
O3' O -0.0852(15) 0.9858(17) 0.6611(11) 0.092(5) Uani 0.551(15) 1 d . . P A 2
O4' O 0.220(3) 0.966(3) 0.5920(19) 0.074(5) Uani 0.551(15) 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 180.0 2_466 . ?
O12 Cu1 N1 89.85(14) 2_466 . ?
O12 Cu1 N1 90.15(14) . . ?
O12 Cu1 N1 90.15(14) 2_466 2_466 ?
O12 Cu1 N1 89.85(14) . 2_466 ?
N1 Cu1 N1 180.0 . 2_466 ?
C3 N1 C2 119.8(4) . . ?
C3 N1 Cu1 119.9(3) . . ?
C2 N1 Cu1 120.3(3) . . ?
N1 C2 C3 119.9(4) . 2_566 ?
N1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 2_566 . ?
N1 C3 C2 120.3(4) . 2_566 ?
N1 C3 H3 119.9 . . ?
C2 C3 H3 119.9 2_566 . ?
C12 N11 C16 123.7(5) . . ?
C12 N11 H11 118(5) . . ?
C16 N11 H11 118(5) . . ?
O12 C12 N11 120.2(5) . . ?
O12 C12 C13 122.2(5) . . ?
N11 C12 C13 117.6(5) . . ?
C12 O12 Cu1 135.9(3) . . ?
C14 C13 C12 117.4(5) . . ?
C14 C13 C17 123.9(5) . . ?
C12 C13 C17 118.8(5) . . ?
C13 C14 C15 122.5(6) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C16 C15 C14 119.1(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 N11 119.6(6) . . ?
C15 C16 H16 120.2 . . ?
N11 C16 H16 120.2 . . ?
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 . . ?
H1A O1W H1B 108(7) . . ?
O3 Cl1 O1 123.5(16) . . ?
O3 Cl1 O4 91.5(14) . . ?
O1 Cl1 O4 127.9(13) . . ?
O3 Cl1 O2 112.0(13) . . ?
O1 Cl1 O2 110.4(14) . . ?
O4 Cl1 O2 84.9(13) . . ?
O1' Cl1 O2' 106.8(10) . . ?
O1' Cl1 O3' 103.8(10) . . ?
O2' Cl1 O3' 99.2(8) . . ?
O1' Cl1 O4' 104.9(12) . . ?
O2' Cl1 O4' 136.9(10) . . ?
O3' Cl1 O4' 100.8(10) . . ?
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 1.943(3) 2_466 ?
Cu1 O12 1.943(3) . ?
Cu1 N1 2.064(4) . ?
Cu1 N1 2.064(4) 2_466 ?
N1 C3 1.315(6) . ?
N1 C2 1.321(6) . ?
C2 C3 1.381(6) 2_566 ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
N11 C12 1.349(7) . ?
N11 C16 1.364(7) . ?
N11 H11 0.82(7) . ?
C12 O12 1.279(6) . ?
C12 C13 1.419(7) . ?
C13 C14 1.367(7) . ?
C13 C17 1.482(9) . ?
C14 C15 1.388(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.323(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O1W H1A 0.84(3) . ?
O1W H1B 0.84(3) . ?
Cl1 O3 1.300(13) . ?
Cl1 O1 1.312(17) . ?
Cl1 O4 1.35(3) . ?
Cl1 O1' 1.407(16) . ?
Cl1 O2 1.431(15) . ?
Cl1 O2' 1.455(10) . ?
Cl1 O3' 1.512(10) . ?
Cl1 O4' 1.51(2) . ?
