#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:42:07 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230571 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/68/7056809.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_7056809
loop_
_publ_author_name
'Khan, Samim'
'Sproules, Stephen'
'Natrajan, Louise S.'
'Harms, Klaus'
'Chattopadhyay, Shouvik'
_publ_section_title
;
 End-on cyanate or end-to-end thiocyanate bridged dinuclear copper(ii)
 complexes with a tridentate Schiff base blocking ligand: synthesis,
 structure and magnetic studies
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1634
_journal_paper_doi               10.1039/C7NJ03990E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C34 H38 Cu2 N6 O2 S2, 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C40 H56 Cu2 N8 O6 S2'
_chemical_formula_weight         936.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-10-16 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.121(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5100(4)
_cell_length_b                   7.1497(3)
_cell_length_c                   19.7873(5)
_cell_measurement_reflns_used    30738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      1.34
_cell_volume                     2153.05(12)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.822
_diffrn_reflns_theta_min         1.533
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.7713
_exptl_absorpt_correction_T_min  0.6202
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XSHAPE/XRED'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0243
_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)+(0.0487P)²+0.4225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3977
_reflns_number_total             4551
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj03990e2.cif
_cod_data_source_block           s137
_cod_depositor_comments
'Adding full bibliography for 7056808--7056809.cif.'
_cod_database_code               7056809
_shelx_shelxl_version_number     2016/6
_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. 
;
_shelx_estimated_absorpt_t_min   0.628
_shelx_estimated_absorpt_t_max   0.741
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu1 Cu 0.44231(2) 0.33764(3) 0.43258(2) 0.02156(7) Uani 1 1 d . .
N1 N 0.34412(9) 0.34982(19) 0.48820(7) 0.0242(3) Uani 1 1 d . .
H1 H 0.3529(12) 0.450(3) 0.5105(10) 0.027(5) Uiso 1 1 d . .
C2 C 0.26176(10) 0.3730(2) 0.43741(8) 0.0257(3) Uani 1 1 d . .
H2A H 0.215002 0.421503 0.460396 0.031 Uiso 1 1 calc R U
H2B H 0.242425 0.250866 0.416211 0.031 Uiso 1 1 calc R U
C3 C 0.27788(10) 0.5089(2) 0.38261(8) 0.0246(3) Uani 1 1 d . .
H3A H 0.226252 0.512997 0.344403 0.030 Uiso 1 1 calc R U
H3B H 0.288055 0.636208 0.402243 0.030 Uiso 1 1 calc R U
N4 N 0.35587(8) 0.44396(17) 0.35716(6) 0.0223(3) Uani 1 1 d . .
C5 C 0.36745(9) 0.4910(2) 0.29609(8) 0.0218(3) Uani 1 1 d . .
C6 C 0.44562(10) 0.4303(2) 0.27071(8) 0.0221(3) Uani 1 1 d . .
C7 C 0.52605(10) 0.4053(2) 0.31694(8) 0.0238(3) Uani 1 1 d . .
O7 O 0.53578(7) 0.39631(16) 0.38417(5) 0.0246(2) Uani 1 1 d . .
C8 C 0.60544(10) 0.3965(2) 0.28943(8) 0.0279(3) Uani 1 1 d . .
H8 H 0.660457 0.392194 0.320372 0.033 Uiso 1 1 calc R U
C9 C 0.60402(10) 0.3941(2) 0.22086(9) 0.0291(3) Uani 1 1 d . .
H9 H 0.657863 0.391719 0.204720 0.035 Uiso 1 1 calc R U
C10 C 0.52300(10) 0.3950(2) 0.17244(8) 0.0254(3) Uani 1 1 d . .
C11 C 0.52133(11) 0.3760(2) 0.10078(8) 0.0290(3) Uani 1 1 d . .
H11 H 0.575117 0.369309 0.084674 0.035 Uiso 1 1 calc R U
C12 C 0.44359(11) 0.3673(2) 0.05459(8) 0.0293(3) Uani 1 1 d . .
H12 H 0.443297 0.356309 0.006702 0.035 Uiso 1 1 calc R U
C13 C 0.36437(11) 0.3746(2) 0.07851(8) 0.0267(3) Uani 1 1 d . .
H13 H 0.310142 0.365598 0.046752 0.032 Uiso 1 1 calc R U
C14 C 0.36450(10) 0.3948(2) 0.14783(8) 0.0245(3) Uani 1 1 d . .
H14 H 0.309960 0.398159 0.162908 0.029 Uiso 1 1 calc R U
C15 C 0.44344(10) 0.4107(2) 0.19725(8) 0.0231(3) Uani 1 1 d . .
C16 C 0.33992(11) 0.1961(2) 0.53809(9) 0.0294(3) Uani 1 1 d . .
H16A H 0.394943 0.196545 0.573093 0.035 Uiso 1 1 calc R U
H16B H 0.336833 0.075297 0.513289 0.035 Uiso 1 1 calc R U
C17 C 0.26255(11) 0.2084(3) 0.57470(9) 0.0341(4) Uani 1 1 d . .
H17A H 0.267696 0.110322 0.609847 0.051 Uiso 1 1 calc R U
H17B H 0.207677 0.191610 0.541212 0.051 Uiso 1 1 calc R U
H17C H 0.262380 0.331227 0.596663 0.051 Uiso 1 1 calc R U
C18 C 0.30454(10) 0.6279(2) 0.25407(8) 0.0247(3) Uani 1 1 d . .
H18A H 0.328571 0.669543 0.214288 0.037 Uiso 1 1 calc R U
H18B H 0.296553 0.736049 0.282640 0.037 Uiso 1 1 calc R U
H18C H 0.247744 0.566646 0.238043 0.037 Uiso 1 1 calc R U
O1L O 0.83802(10) 0.3235(2) 0.38369(9) 0.0612(5) Uani 1 1 d . .
C1L C 0.86138(13) 0.3536(3) 0.32922(12) 0.0465(5) Uani 1 1 d . .
H1L H 0.816778 0.353944 0.288885 0.056 Uiso 1 1 calc R U
N2L N 0.94243(9) 0.3858(2) 0.32077(8) 0.0328(3) Uani 1 1 d . .
C3L C 1.01576(12) 0.3841(3) 0.37904(10) 0.0404(4) Uani 1 1 d . .
H3LA H 1.053424 0.492807 0.376350 0.061 Uiso 1 1 calc R U
H3LB H 1.049921 0.269179 0.377987 0.061 Uiso 1 1 calc R U
H3LC H 0.993315 0.389120 0.422036 0.061 Uiso 1 1 calc R U
C4L C 0.96384(14) 0.4103(3) 0.25306(10) 0.0431(4) Uani 1 1 d . .
H4LA H 0.997024 0.526611 0.252167 0.065 Uiso 1 1 calc R U
H4LB H 0.909517 0.416350 0.218344 0.065 Uiso 1 1 calc R U
H4LC H 0.999446 0.304415 0.242952 0.065 Uiso 1 1 calc R U
H1W H 0.6572(17) 0.280(4) 0.4327(13) 0.056(7) Uiso 1 1 d . .
O1W O 0.70312(9) 0.26830(19) 0.45722(6) 0.0323(3) Uani 1 1 d . .
H2W H 0.7390(16) 0.285(3) 0.4316(12) 0.053(7) Uiso 1 1 d . .
N1' N 0.52879(8) 0.25203(19) 0.51248(7) 0.0250(3) Uani 1 1 d . .
C2' C 0.55841(9) 0.1529(2) 0.55759(8) 0.0235(3) Uani 1 1 d . .
S3' S 0.60025(3) 0.01547(5) 0.62169(2) 0.02710(10) Uani 1 1 d . .
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'
S S 0.1246 0.1234 '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_3
O7 Cu1 N4 90.39(5) .
O7 Cu1 N1' 90.31(5) .
N4 Cu1 N1' 174.96(5) .
O7 Cu1 N1 164.89(5) .
N4 Cu1 N1 85.53(5) .
N1' Cu1 N1 92.52(5) .
O7 Cu1 S3' 98.68(4) 3_656
N4 Cu1 S3' 88.93(4) 3_656
N1' Cu1 S3' 95.89(4) 3_656
N1 Cu1 S3' 95.79(4) 3_656
C2 N1 C16 113.11(12) .
C2 N1 Cu1 105.97(9) .
C16 N1 Cu1 117.27(10) .
C2 N1 H1 107.1(13) .
C16 N1 H1 107.7(13) .
Cu1 N1 H1 104.9(12) .
N1 C2 C3 108.64(12) .
N1 C2 H2A 110.0 .
C3 C2 H2A 110.0 .
N1 C2 H2B 110.0 .
C3 C2 H2B 110.0 .
H2A C2 H2B 108.3 .
N4 C3 C2 107.63(12) .
N4 C3 H3A 110.2 .
C2 C3 H3A 110.2 .
N4 C3 H3B 110.2 .
C2 C3 H3B 110.2 .
H3A C3 H3B 108.5 .
C5 N4 C3 120.41(13) .
C5 N4 Cu1 127.75(10) .
C3 N4 Cu1 110.42(10) .
N4 C5 C6 120.92(13) .
N4 C5 C18 119.23(13) .
C6 C5 C18 119.48(13) .
C7 C6 C15 118.93(13) .
C7 C6 C5 120.19(13) .
C15 C6 C5 120.67(13) .
O7 C7 C6 125.40(13) .
O7 C7 C8 116.21(13) .
C6 C7 C8 118.34(14) .
C7 O7 Cu1 124.28(10) .
C9 C8 C7 121.99(15) .
C9 C8 H8 119.0 .
C7 C8 H8 119.0 .
C8 C9 C10 121.04(14) .
C8 C9 H9 119.5 .
C10 C9 H9 119.5 .
C15 C10 C11 120.27(14) .
C15 C10 C9 118.74(14) .
C11 C10 C9 120.98(14) .
C12 C11 C10 121.07(15) .
C12 C11 H11 119.5 .
C10 C11 H11 119.5 .
C11 C12 C13 119.39(15) .
C11 C12 H12 120.3 .
C13 C12 H12 120.3 .
C14 C13 C12 120.47(15) .
C14 C13 H13 119.8 .
C12 C13 H13 119.8 .
C13 C14 C15 122.03(14) .
C13 C14 H14 119.0 .
C15 C14 H14 119.0 .
C14 C15 C10 116.66(14) .
C14 C15 C6 123.24(13) .
C10 C15 C6 119.99(14) .
N1 C16 C17 114.43(14) .
N1 C16 H16A 108.7 .
C17 C16 H16A 108.7 .
N1 C16 H16B 108.7 .
C17 C16 H16B 108.7 .
H16A C16 H16B 107.6 .
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 .
C5 C18 H18A 109.5 .
C5 C18 H18B 109.5 .
H18A C18 H18B 109.5 .
C5 C18 H18C 109.5 .
H18A C18 H18C 109.5 .
H18B C18 H18C 109.5 .
O1L C1L N2L 126.5(2) .
O1L C1L H1L 116.8 .
N2L C1L H1L 116.8 .
C1L N2L C4L 122.06(18) .
C1L N2L C3L 121.08(17) .
C4L N2L C3L 116.70(15) .
N2L C3L H3LA 109.5 .
N2L C3L H3LB 109.5 .
H3LA C3L H3LB 109.5 .
N2L C3L H3LC 109.5 .
H3LA C3L H3LC 109.5 .
H3LB C3L H3LC 109.5 .
N2L C4L H4LA 109.5 .
N2L C4L H4LB 109.5 .
H4LA C4L H4LB 109.5 .
N2L C4L H4LC 109.5 .
H4LA C4L H4LC 109.5 .
H4LB C4L H4LC 109.5 .
H1W O1W H2W 104(2) .
C2' N1' Cu1 156.29(12) .
N1' C2' S3' 179.33(14) .
C2' S3' Cu1 102.55(5) 3_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O7 1.9317(10) .
Cu1 N4 1.9572(13) .
Cu1 N1' 1.9635(13) .
Cu1 N1 2.0456(13) .
Cu1 S3' 2.7730(4) 3_656
N1 C2 1.4744(19) .
N1 C16 1.487(2) .
N1 H1 0.84(2) .
C2 C3 1.513(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 N4 1.4722(18) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
N4 C5 1.2999(19) .
C5 C6 1.465(2) .
C5 C18 1.512(2) .
C6 C7 1.409(2) .
C6 C15 1.454(2) .
C7 O7 1.3113(18) .
C7 C8 1.441(2) .
C8 C9 1.353(2) .
C8 H8 0.9500 .
C9 C10 1.426(2) .
C9 H9 0.9500 .
C10 C15 1.418(2) .
C10 C11 1.420(2) .
C11 C12 1.367(2) .
C11 H11 0.9500 .
C12 C13 1.400(2) .
C12 H12 0.9500 .
C13 C14 1.379(2) .
C13 H13 0.9500 .
C14 C15 1.417(2) .
C14 H14 0.9500 .
C16 C17 1.519(2) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
O1L C1L 1.221(3) .
C1L N2L 1.320(2) .
C1L H1L 0.9500 .
N2L C4L 1.452(2) .
N2L C3L 1.455(2) .
C3L H3LA 0.9800 .
C3L H3LB 0.9800 .
C3L H3LC 0.9800 .
C4L H4LA 0.9800 .
C4L H4LB 0.9800 .
C4L H4LC 0.9800 .
O1W H1W 0.79(3) .
O1W H2W 0.83(2) .
N1' C2' 1.163(2) .
C2' S3' 1.6366(16) .
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
N1 H1 O1W 0.84(2) 2.33(2) 3.0763(19) 148.3(16) 3_666
O1W H1W O7 0.79(3) 2.11(3) 2.8663(17) 161(3) .
O1W H2W O1L 0.83(2) 1.97(3) 2.7971(19) 171(2) .
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
C16 N1 C2 C3 -170.62(13)
Cu1 N1 C2 C3 -40.81(14)
N1 C2 C3 N4 51.66(16)
C2 C3 N4 C5 156.07(13)
C2 C3 N4 Cu1 -36.47(14)
C3 N4 C5 C6 178.81(13)
Cu1 N4 C5 C6 13.7(2)
C3 N4 C5 C18 5.7(2)
Cu1 N4 C5 C18 -159.39(11)
N4 C5 C6 C7 -31.7(2)
C18 C5 C6 C7 141.40(15)
N4 C5 C6 C15 153.70(14)
C18 C5 C6 C15 -33.2(2)
C15 C6 C7 O7 -171.26(14)
C5 C6 C7 O7 14.0(2)
C15 C6 C7 C8 11.5(2)
C5 C6 C7 C8 -163.17(14)
C6 C7 O7 Cu1 20.2(2)
C8 C7 O7 Cu1 -162.53(11)
O7 C7 C8 C9 176.34(15)
C6 C7 C8 C9 -6.2(2)
C7 C8 C9 C10 -1.8(3)
C8 C9 C10 C15 4.0(2)
C8 C9 C10 C11 -174.46(16)
C15 C10 C11 C12 -1.8(2)
C9 C10 C11 C12 176.62(16)
C10 C11 C12 C13 -0.9(2)
C11 C12 C13 C14 1.5(2)
C12 C13 C14 C15 0.6(2)
C13 C14 C15 C10 -3.2(2)
C13 C14 C15 C6 -179.39(15)
C11 C10 C15 C14 3.8(2)
C9 C10 C15 C14 -174.74(15)
C11 C10 C15 C6 -179.92(14)
C9 C10 C15 C6 1.6(2)
C7 C6 C15 C14 166.64(15)
C5 C6 C15 C14 -18.7(2)
C7 C6 C15 C10 -9.4(2)
C5 C6 C15 C10 165.26(14)
C2 N1 C16 C17 -53.00(19)
Cu1 N1 C16 C17 -176.81(11)
O1L C1L N2L C4L 176.7(2)
O1L C1L N2L C3L 1.4(3)
