#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:09:13 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258819 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705496.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_7705496
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      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
;
2020-07-23 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.399(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.0309(19)
_cell_length_b                   6.8184(5)
_cell_length_c                   7.7006(15)
_cell_measurement_reflns_used    1703
_cell_measurement_temperature    280.0(2)
_cell_measurement_theta_max      76.3600
_cell_measurement_theta_min      5.6510
_cell_volume                     1209.2(3)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      280(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3789
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.645
_diffrn_reflns_theta_min         5.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.681
_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            green
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       prism
_exptl_crystal_F_000             610
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0398
_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)+(0.0726P)²+0.6302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1167
_reflns_number_total             1333
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02716b2.cif
_cod_data_source_block           ekdi7a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct' was changed
to 'direct' 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.

data item '_atom_sites_solution_secondary' value 'Difmap' was changed
to 'difmap' 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               7705496
_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 0.500000 0.500000 0.500000 0.0395(2) Uani 1 4 d S T P . .
N1 N 0.500000 0.7970(3) 0.500000 0.0385(5) Uani 1 2 d S T P . .
C2 C 0.47665(10) 0.8988(3) 0.6305(3) 0.0413(5) Uani 1 1 d . . . . .
H2 H 0.460090 0.831867 0.723004 0.050 Uiso 1 1 calc R U . . .
N11 N 0.35367(13) 0.500000 0.4577(4) 0.0521(7) Uani 1 2 d S T P . .
H11 H 0.376(2) 0.500000 0.373(6) 0.064(13) Uiso 1 2 d S . P . .
C12 C 0.37662(14) 0.500000 0.6205(4) 0.0452(7) Uani 1 2 d S T P . .
O12 O 0.43104(10) 0.500000 0.6441(3) 0.0458(5) Uani 1 2 d S T P . .
C13 C 0.33640(18) 0.500000 0.7587(6) 0.0640(10) Uani 1 2 d S T P . .
H13 H 0.349264 0.500000 0.873475 0.077 Uiso 1 2 calc R U P . .
C14 C 0.27864(19) 0.500000 0.7208(7) 0.0742(12) Uani 1 2 d S T P . .
H14 H 0.252274 0.500000 0.811734 0.089 Uiso 1 2 calc R U P . .
C15 C 0.25779(19) 0.500000 0.5535(7) 0.0732(12) Uani 1 2 d S T P . .
H15 H 0.218018 0.500000 0.531847 0.088 Uiso 1 2 calc R U P . .
C16 C 0.29630(18) 0.500000 0.4190(6) 0.0638(10) Uani 1 2 d S T P . .
C17 C 0.2809(2) 0.500000 0.2301(7) 0.0884(15) Uani 1 2 d S T P . .
H17A H 0.290823 0.375515 0.180201 0.106 Uiso 0.5 1 calc R U P . .
H17B H 0.301945 0.602157 0.172294 0.106 Uiso 0.5 1 calc R U P . .
H17C H 0.239939 0.522328 0.216378 0.106 Uiso 0.5 1 calc R U P . .
O1W O 0.55412(13) 0.500000 0.7802(4) 0.0572(6) Uani 1 2 d DS T P . .
H1 H 0.5558(12) 0.600(3) 0.838(3) 0.053(8) Uiso 1 1 d D . . . .
Cl1 Cl 0.60847(4) 1.000000 0.91575(12) 0.0564(3) Uani 1 2 d S T P . .
O1 O 0.61402(19) 1.000000 0.7338(5) 0.1073(14) Uani 1 2 d S T P A .
O3 O 0.6665(6) 0.943(4) 0.9932(17) 0.070(5) Uani 0.25 1 d . . P A 1
O2 O 0.5891(4) 0.8218(17) 0.9814(18) 0.097(3) Uani 0.5 1 d . . P A 1
O3A O 0.6525(8) 1.059(9) 0.997(4) 0.168(19) Uani 0.25 1 d . . P A 2
O2A O 0.5654(3) 0.8502(15) 0.9614(14) 0.074(2) Uani 0.5 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 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
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 . 5_666 ?
O12 Cu1 N1 90.0 . . ?
O12 Cu1 N1 90.0 5_666 . ?
O12 Cu1 N1 90.0 . 5_666 ?
O12 Cu1 N1 90.0 5_666 5_666 ?
N1 Cu1 N1 180.0 . 5_666 ?
O12 Cu1 O1W 84.91(10) . . ?
O12 Cu1 O1W 95.09(10) 5_666 . ?
N1 Cu1 O1W 90.0 . . ?
N1 Cu1 O1W 90.0 5_666 . ?
C2 N1 C2 117.5(2) 2_656 . ?
C2 N1 Cu1 121.27(12) 2_656 . ?
C2 N1 Cu1 121.27(12) . . ?
N1 C2 C2 121.26(12) . 6_575 ?
N1 C2 H2 119.4 . . ?
C2 C2 H2 119.4 6_575 . ?
C16 N11 C12 125.3(3) . . ?
C16 N11 H11 116(3) . . ?
C12 N11 H11 119(3) . . ?
O12 C12 N11 120.8(3) . . ?
O12 C12 C13 123.0(3) . . ?
N11 C12 C13 116.2(3) . . ?
C12 O12 Cu1 137.0(2) . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 122.5(4) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 119.1(4) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
N11 C16 C15 118.0(4) . . ?
N11 C16 C17 116.1(4) . . ?
C15 C16 C17 125.9(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C17 H17A 109.5(11) . 6_565 ?
H17A C17 H17A 124.3 . 6_565 ?
H17B C17 H17A 18.2 . 6_565 ?
H17C C17 H17A 93.0 . 6_565 ?
C16 C17 H17B 109.5(17) . 6_565 ?
H17A C17 H17B 18.2 . 6_565 ?
H17B C17 H17B 93.0 . 6_565 ?
H17C C17 H17B 124.3 . 6_565 ?
H17A C17 H17B 109.5 6_565 6_565 ?
C16 C17 H17C 109.5(7) . 6_565 ?
H17A C17 H17C 93.0 . 6_565 ?
H17B C17 H17C 124.3 . 6_565 ?
H17C C17 H17C 18.2 . 6_565 ?
H17A C17 H17C 109.5 6_565 6_565 ?
H17B C17 H17C 109.5 6_565 6_565 ?
Cu1 O1W H1 120(2) . . ?
Cu1 O1W H1 120(2) . 6_565 ?
H1 O1W H1 114(4) . 6_565 ?
O2 Cl1 O2 121.8(10) 6_575 . ?
O3A Cl1 O1 114.7(14) . . ?
O3A Cl1 O1 114.7(14) 6_575 . ?
O2 Cl1 O1 113.2(6) 6_575 . ?
O2 Cl1 O1 113.2(6) . . ?
O3A Cl1 O2A 102(2) . 6_575 ?
O3A Cl1 O2A 130(2) 6_575 6_575 ?
O2 Cl1 O2A 24.0(5) 6_575 6_575 ?
O2 Cl1 O2A 107.6(4) . 6_575 ?
O1 Cl1 O2A 107.7(4) . 6_575 ?
O3A Cl1 O2A 130(2) . . ?
O3A Cl1 O2A 102(2) 6_575 . ?
O1 Cl1 O2A 107.7(4) . . ?
O2A Cl1 O2A 88.1(6) 6_575 . ?
O2 Cl1 O3 111.4(10) 6_575 . ?
O2 Cl1 O3 85.3(10) . . ?
O1 Cl1 O3 107.9(5) . . ?
O2 Cl1 O3 85.3(10) 6_575 6_575 ?
O2 Cl1 O3 111.4(10) . 6_575 ?
O1 Cl1 O3 107.9(5) . 6_575 ?
O3 Cl1 O3 29.6(19) . 6_575 ?
O3 O3 Cl1 75.2(9) 6_575 . ?
O3A O3A Cl1 71(3) 6_575 . ?
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(2) . ?
Cu1 O12 1.944(2) 5_666 ?
Cu1 N1 2.025(2) . ?
Cu1 N1 2.025(2) 5_666 ?
Cu1 O1W 2.485(3) . ?
N1 C2 1.337(2) 2_656 ?
N1 C2 1.337(2) . ?
C2 C2 1.381(4) 6_575 ?
C2 H2 0.9300 . ?
N11 C16 1.353(5) . ?
N11 C12 1.357(5) . ?
N11 H11 0.83(5) . ?
C12 O12 1.265(4) . ?
C12 C13 1.416(5) . ?
C13 C14 1.360(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.371(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.369(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.495(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 H17A 0.96(5) 6_565 ?
C17 H17B 0.96(8) 6_565 ?
C17 H17C 0.96(3) 6_565 ?
O1W H1 0.818(17) . ?
O1W H1 0.818(17) 6_565 ?
Cl1 O3A 1.25(3) . ?
Cl1 O3A 1.25(3) 6_575 ?
Cl1 O2 1.390(12) 6_575 ?
Cl1 O2 1.390(12) . ?
Cl1 O1 1.408(4) . ?
Cl1 O2A 1.468(10) 6_575 ?
Cl1 O2A 1.468(10) . ?
Cl1 O3 1.509(15) . ?
Cl1 O3 1.509(15) 6_575 ?
O3 O3 0.77(5) 6_575 ?
O3A O3A 0.80(12) 6_575 ?
