#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:09:13 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258819 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705495.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_7705495
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
_chemical_name_systematic
' catena-diaqua-bis(6-methyl-2-pyridone)(u/-pyrazine)copper(II) perchlorate'
_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     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
_cell_angle_beta                 90.189(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.016(11)
_cell_length_b                   6.822(3)
_cell_length_c                   7.656(4)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.4755
_cell_measurement_theta_min      3.1146
_cell_volume                     1202.1(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Saturn70 (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6233
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.207
_diffrn_reflns_theta_min         3.114
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7581
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            'Light Green'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       Prism
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.410
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0380
_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)+(0.0610P)²+1.8123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1670
_reflns_number_total             1686
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02716b2.cif
_cod_data_source_block           vsa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705494--7705499.cif.
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7705495
_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'
'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
Cu1 Cu 0.000000 0.000000 0.000000 0.01690(15) Uani 1 4 d S T P . .
N1 N 0.000000 -0.2965(3) 0.000000 0.0168(4) Uani 1 2 d S T P . .
C2 C -0.02277(7) -0.3984(2) 0.1329(2) 0.0192(3) Uani 1 1 d . . . . .
H2 H -0.039231 -0.330108 0.228853 0.023 Uiso 1 1 calc R U . . .
N11 N 0.14622(10) 0.000000 0.0343(3) 0.0255(4) Uani 1 2 d S T P . .
H11 H 0.1214(16) 0.000000 0.123(5) 0.031 Uiso 1 2 d S U P . .
C12 C 0.12298(11) 0.000000 -0.1287(3) 0.0213(4) Uani 1 2 d S T P . .
O12 O 0.06813(8) 0.000000 -0.1515(2) 0.0216(3) Uani 1 2 d S T P . .
C13 C 0.16268(12) 0.000000 -0.2693(4) 0.0309(6) Uani 1 2 d S T P . .
H13 H 0.148895 0.000000 -0.386446 0.037 Uiso 1 2 calc R U P . .
C14 C 0.22121(13) 0.000000 -0.2354(5) 0.0381(7) Uani 1 2 d S T P . .
H14 H 0.247729 0.000000 -0.330201 0.046 Uiso 1 2 calc R U P . .
C15 C 0.24275(13) 0.000000 -0.0646(5) 0.0372(7) Uani 1 2 d S T P . .
H15 H 0.283448 0.000000 -0.043459 0.045 Uiso 1 2 calc R U P . .
C16 C 0.20456(12) 0.000000 0.0717(4) 0.0329(6) Uani 1 2 d S T P . .
C17 C 0.22043(17) 0.000000 0.2610(5) 0.0473(9) Uani 1 2 d S T P . .
H17A H 0.2038(14) -0.108(6) 0.317(4) 0.057 Uiso 1 1 d . U . . .
H17C H 0.256(2) 0.000000 0.271(7) 0.057 Uiso 1 2 d S U P . .
O1W O 0.05612(9) 0.000000 0.2756(3) 0.0272(4) Uani 1 2 d S T P . .
H1W H 0.0590(12) 0.089(4) 0.339(4) 0.033 Uiso 1 1 d . U . . .
Cl1 Cl 0.39243(3) 0.000000 -0.41446(8) 0.02683(18) Uani 1 2 d S T P . .
O1 O 0.38681(12) 0.000000 -0.2287(3) 0.0515(7) Uani 1 2 d S T P A .
O2 O 0.42515(14) 0.1657(3) -0.4698(3) 0.0785(9) Uani 1 1 d . . . . .
O3 O 0.33842(14) 0.0564(7) -0.4926(5) 0.0613(18) Uani 0.5 1 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 0.0033 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(6) 5 . ?
O12 Cu1 N1 90.0 5 . ?
O12 Cu1 N1 90.0 . . ?
O12 Cu1 N1 90.0 5 5 ?
O12 Cu1 N1 90.0 . 5 ?
N1 Cu1 N1 180.0 . 5 ?
O12 Cu1 O1W 84.91(8) 5 . ?
O12 Cu1 O1W 95.09(8) . . ?
N1 Cu1 O1W 90.0 . . ?
N1 Cu1 O1W 90.0 5 . ?
C2 N1 C2 117.5(2) . 2 ?
C2 N1 Cu1 121.25(10) . . ?
C2 N1 Cu1 121.25(10) 2 . ?
N1 C2 C2 121.26(10) . 6_545 ?
N1 C2 H2 119.4 . . ?
C2 C2 H2 119.4 6_545 . ?
C12 N11 C16 125.1(2) . . ?
C12 N11 H11 117(2) . . ?
C16 N11 H11 118(2) . . ?
O12 C12 N11 120.9(2) . . ?
O12 C12 C13 122.6(2) . . ?
N11 C12 C13 116.5(2) . . ?
C12 O12 Cu1 135.71(17) . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 121.5(3) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 N11 118.2(3) . . ?
C15 C16 C17 125.8(3) . . ?
N11 C16 C17 116.0(3) . . ?
C16 C17 H17A 110(2) . . ?
C16 C17 H17C 109(4) . . ?
H17A C17 H17C 111(3) . . ?
C16 C17 H17A 110(2) . 6 ?
H17A C17 H17A 104(4) . 6 ?
H17C C17 H17A 111(3) . 6 ?
Cu1 O1W H1W 125(2) . . ?
Cu1 O1W H1W 125(2) . 6 ?
H1W O1W H1W 102(4) . 6 ?
O2 Cl1 O2 105.1(2) 6 . ?
O2 Cl1 O1 110.25(11) 6 . ?
O2 Cl1 O1 110.25(11) . . ?
O2 Cl1 O3 97.0(2) 6 6 ?
O2 Cl1 O3 123.3(2) . 6 ?
O1 Cl1 O3 109.6(2) . 6 ?
O2 Cl1 O3 123.3(2) 6 . ?
O2 Cl1 O3 97.0(2) . . ?
O1 Cl1 O3 109.6(2) . . ?
O3 Cl1 O3 31.2(4) 6 . ?
O3 O3 Cl1 74.4(2) 6 . ?
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 1.9536(19) 5 ?
Cu1 O12 1.9536(19) . ?
Cu1 N1 2.023(2) . ?
Cu1 N1 2.023(2) 5 ?
Cu1 O1W 2.470(2) . ?
N1 C2 1.3404(19) . ?
N1 C2 1.3404(19) 2 ?
C2 C2 1.386(3) 6_545 ?
C2 H2 0.9500 . ?
N11 C12 1.357(3) . ?
N11 C16 1.372(4) . ?
N11 H11 0.89(4) . ?
C12 O12 1.274(3) . ?
C12 C13 1.414(4) . ?
C13 C14 1.371(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.397(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.367(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.494(5) . ?
C17 H17A 0.93(4) . ?
C17 H17C 0.83(5) . ?
C17 H17A 0.93(4) 6 ?
O1W H1W 0.78(3) . ?
O1W H1W 0.78(3) 6 ?
Cl1 O2 1.424(2) 6 ?
Cl1 O2 1.424(2) . ?
Cl1 O1 1.429(2) . ?
Cl1 O3 1.431(3) 6 ?
Cl1 O3 1.431(3) . ?
O3 O3 0.770(10) 6 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2 O12 0.95 2.42 2.915(2) 112.1 5 yes
C2 H2 O2 0.95 2.45 3.302(3) 149.1 3_446 yes
N11 H11 O1W 0.89(4) 1.91(4) 2.782(3) 168(4) . yes
C17 H17C O3a 0.83(5) 2.64(5) 3.324(5) 141(4) 1_556 yes
C17 H17C O3a 0.83(5) 2.64(5) 3.324(5) 141(4) 6_556 yes
O1W H1W O2 0.78(3) 1.98(3) 2.756(3) 170(3) 7 yes
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
C2 N1 C2 C2 0.004(0) 2 . . 6_545 ?
Cu1 N1 C2 C2 180.002(1) . . . 6_545 ?
C16 N11 C12 O12 180.0 . . . . ?
C16 N11 C12 C13 0.000(0) . . . . ?
N11 C12 O12 Cu1 0.000(0) . . . . ?
C13 C12 O12 Cu1 180.000(0) . . . . ?
O12 C12 C13 C14 180.000(0) . . . . ?
N11 C12 C13 C14 0.000(0) . . . . ?
C12 C13 C14 C15 0.000(0) . . . . ?
C13 C14 C15 C16 0.000(0) . . . . ?
C14 C15 C16 N11 0.000(0) . . . . ?
C14 C15 C16 C17 180.000(0) . . . . ?
C12 N11 C16 C15 0.000(0) . . . . ?
C12 N11 C16 C17 180.000(0) . . . . ?
O2 Cl1 O3 O3 36.59(14) 6 . . 6 ?
O2 Cl1 O3 O3 149.86(11) . . . 6 ?
O1 Cl1 O3 O3 -95.70(9) . . . 6 ?
