#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:21:30 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193850 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/18/7041834.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_7041834
loop_
_publ_author_name
'Singh, Yogendra Pratap'
'Patel, Ram N.'
'Singh, Yogendra'
'Choquesillo-Lazarte, Duane'
'Butcher, R. J.'
_publ_section_title
;
 Classical hydrogen bonding and stacking of chelate rings in new
 copper(ii) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2803
_journal_page_last               2820
_journal_paper_doi               10.1039/c6dt04661d
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C28 H22 Cl2 Cu2 N8 O2, 2(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C28 H30 Cl4 Cu2 N8 O14'
_chemical_formula_weight         971.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-03 deposited with the CCDC.
2017-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                107.849(5)
_cell_angle_beta                 97.174(5)
_cell_angle_gamma                94.306(4)
_cell_formula_units_Z            1
_cell_length_a                   6.9846(4)
_cell_length_b                   11.4155(5)
_cell_length_c                   12.6028(8)
_cell_measurement_reflns_used    2846
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      71.0439
_cell_measurement_theta_min      3.7271
_cell_volume                     942.14(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'SHELXT (Sheldrick, 2008)'
_computing_publication_material  'SHELXT (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Shelxt (Shedlrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6047
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         71.183
_diffrn_reflns_theta_min         4.098
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
blue-green
;
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description
;
prism
;
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0609
_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)+(0.1311P)²+0.2165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3021
_reflns_number_total             3546
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04661d3.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7041832--7041834.cif.'
_cod_original_cell_volume        942.14(9)
_cod_database_code               7041834
_shelx_shelxl_version_number     2014/7
_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 0.05374(6) 0.22564(4) 0.87838(4) 0.04410(16) Uani 1 1 d . . . . .
Cl1 Cl 0.54376(13) 0.83492(8) 1.20301(8) 0.0598(2) Uani 1 1 d . . . . .
O1 O 0.1772(4) 0.3205(2) 1.0235(2) 0.0507(6) Uani 1 1 d . . . . .
N1 N -0.0686(4) 0.1386(3) 0.7202(2) 0.0467(6) Uani 1 1 d . . . . .
N2 N 0.0816(4) 0.3643(2) 0.8212(2) 0.0421(6) Uani 1 1 d . . . . .
C6 C 0.1607(5) 0.4768(3) 0.8755(3) 0.0447(7) Uani 1 1 d . . . . .
H3 H 0.1610 0.5346 0.8371 0.054 Uiso 1 1 calc R U . . .
N4 N 0.0164(4) 0.0868(2) 0.9439(2) 0.0463(6) Uani 1 1 d . . . . .
C1 C -0.1443(5) 0.0184(3) 0.6699(3) 0.0548(8) Uani 1 1 d . . . . .
H1 H -0.1341 -0.0362 0.7114 0.066 Uiso 1 1 calc R U . . .
C2 C -0.2350(6) -0.0252(4) 0.5606(4) 0.0642(10) Uani 1 1 d . . . . .
H2 H -0.2854 -0.1082 0.5282 0.077 Uiso 1 1 calc R U . . .
C3 C -0.2507(6) 0.0554(4) 0.4993(3) 0.0682(11) Uani 1 1 d . . . . .
H3A H -0.3150 0.0272 0.4253 0.082 Uiso 1 1 calc R U . . .
C4 C -0.1727(6) 0.1772(4) 0.5461(3) 0.0635(10) Uani 1 1 d . . . . .
H4 H -0.1817 0.2320 0.5047 0.076 Uiso 1 1 calc R U . . .
C5 C -0.0789(5) 0.2163(3) 0.6582(3) 0.0474(7) Uani 1 1 d . . . . .
N3 N 0.0055(4) 0.3344(3) 0.7097(2) 0.0513(7) Uani 1 1 d . . . . .
H6 H 0.0108 0.3877 0.6742 0.062 Uiso 1 1 calc R U . . .
C7 C 0.2476(4) 0.5166(3) 0.9918(3) 0.0424(6) Uani 1 1 d . . . . .
C8 C 0.3344(5) 0.6390(3) 1.0388(3) 0.0455(7) Uani 1 1 d . . . . .
H8 H 0.3310 0.6915 0.9950 0.055 Uiso 1 1 calc R U . . .
C9 C 0.4248(5) 0.6829(3) 1.1490(3) 0.0491(8) Uani 1 1 d . . . . .
C10 C 0.4301(5) 0.6062(3) 1.2161(3) 0.0515(8) Uani 1 1 d . . . . .
H10 H 0.4914 0.6365 1.2907 0.062 Uiso 1 1 calc R U . . .
C11 C 0.3454(5) 0.4865(3) 1.1723(3) 0.0527(8) Uani 1 1 d . . . . .
H11 H 0.3491 0.4362 1.2181 0.063 Uiso 1 1 calc R U . . .
C12 C 0.2520(5) 0.4366(3) 1.0590(3) 0.0436(7) Uani 1 1 d . . . . .
C13 C 0.1696(5) 0.0651(3) 1.0066(3) 0.0524(8) Uani 1 1 d . . . . .
H13 H 0.2901 0.1095 1.0133 0.063 Uiso 1 1 calc R U . . .
C14 C -0.1536(5) 0.0214(3) 0.9382(3) 0.0502(8) Uani 1 1 d . . . . .
H14 H -0.2639 0.0347 0.8958 0.060 Uiso 1 1 calc R U . . .
Cl2 Cl 0.3313(4) 0.8052(2) 0.76685(19) 0.0670(5) Uani 0.714(4) 1 d D U P A 1
O11 O 0.2958(13) 0.6749(6) 0.7233(8) 0.152(3) Uani 0.714(4) 1 d D U P A 1
O12 O 0.1788(11) 0.8688(8) 0.7412(6) 0.148(3) Uani 0.714(4) 1 d D U P A 1
O13 O 0.4897(11) 0.8432(7) 0.7229(6) 0.150(3) Uani 0.714(4) 1 d D U P A 1
O14 O 0.3867(11) 0.8437(8) 0.8860(5) 0.124(2) Uani 0.714(4) 1 d D U P A 1
Cl2A Cl 0.2836(10) 0.7901(5) 0.7648(5) 0.0670(5) Uani 0.286(4) 1 d D . P A 2
O11A O 0.316(3) 0.7043(13) 0.6627(13) 0.152(3) Uani 0.286(4) 1 d D . P A 2
O12A O 0.0904(17) 0.7658(17) 0.7775(14) 0.148(3) Uani 0.286(4) 1 d D . P A 2
O13A O 0.309(3) 0.9087(12) 0.7535(16) 0.150(3) Uani 0.286(4) 1 d D . P A 2
O14A O 0.409(2) 0.7833(18) 0.8549(12) 0.124(2) Uani 0.286(4) 1 d D . P A 2
O1W O -0.0643(9) 0.5234(5) 0.6043(4) 0.1247(16) Uani 1 1 d D U . . .
H1W1 H 0.026(5) 0.485(5) 0.576(5) 0.187 Uiso 1 1 d D U . . .
H1W2 H -0.155(5) 0.467(4) 0.590(7) 0.187 Uiso 1 1 d D U . . .
O2W O 0.5942(18) 0.6105(15) 0.5402(12) 0.321(6) Uani 1 1 d D U . . .
H2W1 H 0.691(7) 0.653(7) 0.585(6) 0.482 Uiso 1 1 d D U . . .
H2W2 H 0.643(10) 0.558(6) 0.494(5) 0.482 Uiso 1 1 d D U . . .
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
O1 Cu1 N2 92.67(10) . .
O1 Cu1 N1 174.58(11) . .
N2 Cu1 N1 82.00(11) . .
O1 Cu1 N4 85.79(11) . .
N2 Cu1 N4 176.90(11) . .
N1 Cu1 N4 99.59(12) . .
C12 O1 Cu1 128.3(2) . .
C5 N1 C1 118.3(3) . .
C5 N1 Cu1 111.8(2) . .
C1 N1 Cu1 129.8(3) . .
C6 N2 N3 119.1(3) . .
C6 N2 Cu1 128.0(2) . .
N3 N2 Cu1 112.9(2) . .
N2 C6 C7 123.3(3) . .
N2 C6 H3 118.4 . .
C7 C6 H3 118.4 . .
C13 N4 C14 116.8(3) . .
C13 N4 Cu1 117.8(2) . .
C14 N4 Cu1 125.2(2) . .
N1 C1 C2 122.4(4) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C1 C2 C3 118.9(4) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C4 C3 C2 120.7(4) . .
C4 C3 H3A 119.6 . .
C2 C3 H3A 119.6 . .
C3 C4 C5 117.8(4) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
N1 C5 N3 116.8(3) . .
N1 C5 C4 121.8(3) . .
N3 C5 C4 121.4(3) . .
C5 N3 N2 116.4(3) . .
C5 N3 H6 121.8 . .
N2 N3 H6 121.8 . .
C8 C7 C12 119.6(3) . .
C8 C7 C6 117.4(3) . .
C12 C7 C6 123.0(3) . .
C9 C8 C7 120.7(3) . .
C9 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
C8 C9 C10 120.5(3) . .
C8 C9 Cl1 119.4(3) . .
C10 C9 Cl1 120.0(3) . .
C11 C10 C9 119.9(3) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 121.8(3) . .
C10 C11 H11 119.1 . .
C12 C11 H11 119.1 . .
O1 C12 C11 117.7(3) . .
O1 C12 C7 124.7(3) . .
C11 C12 C7 117.5(3) . .
N4 C13 C14 121.6(3) . 2_557
N4 C13 H13 119.2 . .
C14 C13 H13 119.2 2_557 .
N4 C14 C13 121.6(3) . 2_557
N4 C14 H14 119.2 . .
C13 C14 H14 119.2 2_557 .
O12 Cl2 O13 107.1(5) . .
O12 Cl2 O11 115.7(6) . .
O13 Cl2 O11 107.9(5) . .
O12 Cl2 O14 108.9(4) . .
O13 Cl2 O14 106.6(5) . .
O11 Cl2 O14 110.2(5) . .
O14A Cl2A O12A 111.2(11) . .
O14A Cl2A O13A 110.9(11) . .
O12A Cl2A O13A 107.8(10) . .
O14A Cl2A O11A 111.4(11) . .
O12A Cl2A O11A 108.2(10) . .
O13A Cl2A O11A 107.2(10) . .
H1W1 O1W H1W2 103(3) . .
H2W1 O2W H2W2 103(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.874(2) .
Cu1 N2 1.937(3) .
Cu1 N1 1.981(3) .
Cu1 N4 2.014(3) .
Cl1 C9 1.755(3) .
O1 C12 1.305(4) .
N1 C5 1.350(5) .
N1 C1 1.355(5) .
N2 C6 1.298(4) .
N2 N3 1.365(4) .
C6 C7 1.431(4) .
C6 H3 0.9300 .
N4 C13 1.334(4) .
N4 C14 1.336(4) .
C1 C2 1.364(5) .
C1 H1 0.9300 .
C2 C3 1.373(7) .
C2 H2 0.9300 .
C3 C4 1.371(6) .
C3 H3A 0.9300 .
C4 C5 1.401(5) .
C4 H4 0.9300 .
C5 N3 1.355(4) .
N3 H6 0.8600 .
C7 C8 1.396(4) .
C7 C12 1.423(5) .
C8 C9 1.374(5) .
C8 H8 0.9300 .
C9 C10 1.391(5) .
C10 C11 1.363(5) .
C10 H10 0.9300 .
C11 C12 1.415(5) .
C11 H11 0.9300 .
C13 C14 1.377(5) 2_557
C13 H13 0.9300 .
C14 C13 1.377(5) 2_557
C14 H14 0.9300 .
Cl2 O12 1.393(6) .
Cl2 O13 1.396(7) .
Cl2 O11 1.409(6) .
Cl2 O14 1.422(6) .
Cl2A O14A 1.368(12) .
Cl2A O12A 1.396(13) .
Cl2A O13A 1.405(12) .
Cl2A O11A 1.415(13) .
O1W H1W1 0.85(2) .
O1W H1W2 0.830(19) .
O2W H2W1 0.83(2) .
O2W H2W2 0.83(2) .
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
C1 H1 O12 0.93 2.55 3.136(7) 121.5 1_545
C4 H4 O11A 0.93 2.53 3.388(19) 153.4 2_566
N3 H6 O1W 0.86 2.07 2.901(6) 161.3 .
C8 H8 O14 0.93 2.56 3.480(9) 169.8 .
C8 H8 O14A 0.93 2.41 3.296(19) 159.7 .
C13 H13 O14 0.93 2.38 3.182(8) 143.8 2_667
C13 H13 O14A 0.93 2.49 3.289(17) 144.7 2_667
C14 H14 Cl1 0.93 2.93 3.812(4) 159.9 2_567
O1W H1W1 O1W 0.85(2) 2.29(7) 2.793(10) 118(6) 2_566
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_4
N2 Cu1 O1 C12 -1.6(3) .
N4 Cu1 O1 C12 -178.9(3) .
N3 N2 C6 C7 -178.8(3) .
Cu1 N2 C6 C7 1.4(5) .
C5 N1 C1 C2 -2.0(5) .
Cu1 N1 C1 C2 175.8(3) .
N1 C1 C2 C3 -0.2(6) .
C1 C2 C3 C4 1.5(7) .
C2 C3 C4 C5 -0.7(6) .
C1 N1 C5 N3 -177.3(3) .
Cu1 N1 C5 N3 4.6(4) .
C1 N1 C5 C4 2.9(5) .
Cu1 N1 C5 C4 -175.2(3) .
C3 C4 C5 N1 -1.6(6) .
C3 C4 C5 N3 178.6(4) .
N1 C5 N3 N2 -3.9(5) .
C4 C5 N3 N2 175.9(3) .
C6 N2 N3 C5 -178.6(3) .
Cu1 N2 N3 C5 1.2(4) .
N2 C6 C7 C8 177.5(3) .
N2 C6 C7 C12 -1.2(5) .
C12 C7 C8 C9 0.3(5) .
C6 C7 C8 C9 -178.4(3) .
C7 C8 C9 C10 -0.5(5) .
C7 C8 C9 Cl1 176.6(2) .
C8 C9 C10 C11 0.1(5) .
Cl1 C9 C10 C11 -176.9(3) .
C9 C10 C11 C12 0.4(5) .
Cu1 O1 C12 C11 -177.4(2) .
Cu1 O1 C12 C7 2.1(5) .
C10 C11 C12 O1 179.0(3) .
C10 C11 C12 C7 -0.6(5) .
C8 C7 C12 O1 -179.3(3) .
C6 C7 C12 O1 -0.6(5) .
C8 C7 C12 C11 0.2(5) .
C6 C7 C12 C11 178.9(3) .
C14 N4 C13 C14 0.6(6) 2_557
Cu1 N4 C13 C14 174.9(3) 2_557
C13 N4 C14 C13 -0.6(6) 2_557
Cu1 N4 C14 C13 -174.4(3) 2_557
