#------------------------------------------------------------------------------
#$Date: 2019-04-11 01:00:53 +0300 (Thu, 11 Apr 2019) $
#$Revision: 214589 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/32/7123289.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_7123289
loop_
_publ_author_name
'Nagarkar, Sanjog S.'
'Kurasho, Haruna'
'Duong, Nghia Tuan Tuan'
'Nishiyama, Yusuke'
'Kitagawa, Susumu'
'Horike, Satoshi'
_publ_section_title
;
 Crystal Melting and Glass Formation in Copper Thiocyanate based
 Coordination Polymers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02172H
_journal_year                    2019
_chemical_formula_moiety         'C15 H13 Cu2 N5 S3'
_chemical_formula_sum            'C15 H13 Cu2 N5 S3'
_chemical_formula_weight         486.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9442(18)
_cell_length_b                   11.887(2)
_cell_length_c                   27.698(5)
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.3574
_cell_volume                     3603.3(11)
_computing_cell_refinement       'CrystalClear	(Rigaku Inc. 2008)'
_computing_data_collection       'CrystalClear	(Rigaku Inc. 2008)'
_computing_data_reduction        'CrystalClear	(Rigaku Inc. 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.35
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.6126
_exptl_absorpt_correction_T_min  0.6126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0670
_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)+(0.0754P)²+12.2923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3526
_reflns_number_total             4123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc02172h2.cif
_cod_data_source_block           1_C2
_cod_original_cell_volume        3603.2(11)
_cod_database_code               7123289
_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.
;
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.613
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Cu1 Cu 0.80045(6) 0.06923(5) -0.09502(2) 0.0334(2) Uani 1 1 d .
Cu2 Cu 0.46006(7) 0.45161(6) -0.09052(2) 0.0421(2) Uani 1 1 d .
S1 S 0.64274(12) 0.42482(9) -0.14700(4) 0.0291(3) Uani 1 1 d .
S2 S 0.49647(12) 0.64896(10) -0.07099(5) 0.0337(3) Uani 1 1 d .
S3 S 0.22163(13) 0.42517(12) -0.22884(5) 0.0407(4) Uani 1 1 d .
N1 N 0.7135(4) 0.0216(3) -0.03350(15) 0.0289(9) Uani 1 1 d .
C1 C 0.6969(4) 0.3000(4) -0.12999(16) 0.0261(9) Uani 1 1 d .
N2 N 0.7323(4) 0.2108(3) -0.12049(16) 0.0343(10) Uani 1 1 d .
C2 C 0.4934(4) 0.0013(4) 0.13106(18) 0.0299(10) Uani 1 1 d .
H2 H 0.4656 0.0692 0.1167 0.036 Uiso 1 1 calc R
N3 N 0.5190(4) 0.6242(3) 0.02991(16) 0.0328(9) Uani 1 1 d .
C3 C 0.5095(4) 0.6346(4) -0.01181(18) 0.0287(10) Uani 1 1 d .
C4 C 0.6686(5) -0.1169(4) 0.02721(18) 0.0309(10) Uani 1 1 d .
H4 H 0.6689 -0.1937 0.0366 0.037 Uiso 1 1 calc R
N4 N 0.3339(5) 0.4447(4) -0.13865(18) 0.0424(11) Uani 1 1 d .
C5 C 0.6172(5) -0.1631(4) 0.12997(19) 0.0339(11) Uani 1 1 d .
H5 H 0.6767 -0.2100 0.1152 0.041 Uiso 1 1 calc R
C6 C 0.5781(5) -0.0655(4) 0.10666(18) 0.0286(10) Uani 1 1 d .
C7 C 0.7122(5) -0.0851(4) -0.01771(18) 0.0303(10) Uani 1 1 d .
H7 H 0.7428 -0.1420 -0.0385 0.036 Uiso 1 1 calc R
C8 C 0.4498(5) -0.0298(4) 0.17546(19) 0.0344(11) Uani 1 1 d .
H8 H 0.3930 0.0173 0.1917 0.041 Uiso 1 1 calc R
N5 N 0.4864(4) -0.1259(4) 0.19630(15) 0.0330(9) Uani 1 1 d .
C9 C 0.2862(5) 0.4381(4) -0.17596(19) 0.0318(11) Uani 1 1 d .
C10 C 0.6247(4) -0.0347(4) 0.05831(18) 0.0275(10) Uani 1 1 d .
C11 C 0.6686(5) 0.0991(4) -0.00343(19) 0.0330(11) Uani 1 1 d .
H11 H 0.6663 0.1750 -0.0141 0.040 Uiso 1 1 calc R
C12 C 0.5252(7) -0.1709(7) 0.2827(2) 0.071(2) Uani 1 1 d .
H12A H 0.5870 -0.2276 0.2748 0.107 Uiso 1 1 calc GR
H12B H 0.4839 -0.1919 0.3128 0.107 Uiso 1 1 calc GR
H12C H 0.5648 -0.0975 0.2868 0.107 Uiso 1 1 calc GR
C13 C 0.6253(5) 0.0752(4) 0.0421(2) 0.0343(11) Uani 1 1 d .
H13 H 0.5960 0.1340 0.0623 0.041 Uiso 1 1 calc R
C14 C 0.5693(5) -0.1916(4) 0.17458(19) 0.0363(11) Uani 1 1 d .
H14 H 0.5957 -0.2587 0.1900 0.044 Uiso 1 1 calc R
C15 C 0.4340(6) -0.1641(5) 0.2429(2) 0.0502(15) Uani 1 1 d .
H15A H 0.3967 -0.2392 0.2383 0.060 Uiso 1 1 calc R
H15B H 0.3682 -0.1115 0.2525 0.060 Uiso 1 1 calc R
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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 '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
S1 Cu1 Cu2 56.15(4) 7_755 7_755
S1 Cu1 S2 101.91(5) 7_755 7_755
S2 Cu1 Cu2 52.04(4) 7_755 7_755
N1 Cu1 Cu2 104.27(12) . 7_755
N1 Cu1 S1 116.03(12) . 7_755
N1 Cu1 S2 107.32(12) . 7_755
N2 Cu1 Cu2 138.60(13) . 7_755
N2 Cu1 S1 120.66(13) . 7_755
N2 Cu1 S2 96.20(13) . 7_755
N2 Cu1 N1 111.14(18) . .
S1 Cu2 Cu1 49.00(3) . 7_765
S2 Cu2 Cu1 54.08(4) . 7_765
S2 Cu2 S1 97.33(5) . .
N3 Cu2 Cu1 98.76(13) 5_665 7_765
N3 Cu2 S1 112.52(13) 5_665 .
N3 Cu2 S2 103.78(13) 5_665 .
N3 Cu2 N4 132.3(2) 5_665 .
N4 Cu2 Cu1 128.66(16) . 7_765
N4 Cu2 S1 97.58(15) . .
N4 Cu2 S2 108.21(15) . .
Cu1 S1 Cu2 74.84(4) 7_765 .
C1 S1 Cu1 112.78(16) . 7_765
C1 S1 Cu2 102.47(16) . .
Cu2 S2 Cu1 73.88(4) . 7_765
C3 S2 Cu1 98.48(17) . 7_765
C3 S2 Cu2 97.73(17) . .
C7 N1 Cu1 122.8(3) . .
C11 N1 Cu1 120.2(3) . .
C11 N1 C7 116.4(4) . .
N2 C1 S1 176.3(4) . .
C1 N2 Cu1 171.3(4) . .
C8 C2 C6 120.8(5) . .
C3 N3 Cu2 157.9(4) . 5_665
N3 C3 S2 179.8(5) . .
C7 C4 C10 119.0(4) . .
C9 N4 Cu2 160.8(5) . .
C14 C5 C6 120.0(5) . .
C2 C6 C10 121.8(4) . .
C5 C6 C2 116.9(5) . .
C5 C6 C10 121.3(4) . .
N1 C7 C4 123.7(4) . .
N5 C8 C2 120.8(5) . .
C8 N5 C15 121.3(5) . .
C14 N5 C8 120.4(4) . .
C14 N5 C15 118.3(5) . .
N4 C9 S3 178.2(5) . .
C4 C10 C6 120.5(4) . .
C13 C10 C4 117.5(5) . .
C13 C10 C6 122.0(4) . .
N1 C11 C13 123.8(4) . .
C11 C13 C10 119.6(5) . .
N5 C14 C5 121.0(5) . .
N5 C15 C12 113.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu2 2.9733(11) 7_755
Cu1 S1 2.3250(14) 7_755
Cu1 S2 2.5062(15) 7_755
Cu1 N1 2.032(4) .
Cu1 N2 1.971(4) .
Cu2 Cu1 2.9732(11) 7_765
Cu2 S1 2.5584(15) .
Cu2 S2 2.4402(15) .
Cu2 N3 1.919(4) 5_665
Cu2 N4 1.921(5) .
S1 Cu1 2.3250(14) 7_765
S1 C1 1.665(5) .
S2 Cu1 2.5063(15) 7_765
S2 C3 1.654(5) .
S3 C9 1.633(5) .
N1 C7 1.342(6) .
N1 C11 1.336(6) .
C1 N2 1.160(6) .
C2 C6 1.395(7) .
C2 C8 1.370(7) .
N3 Cu2 1.919(4) 5_665
N3 C3 1.167(6) .
C4 C7 1.385(7) .
C4 C10 1.388(7) .
N4 C9 1.161(7) .
C5 C6 1.395(7) .
C5 C14 1.384(7) .
C6 C10 1.479(7) .
C8 N5 1.341(7) .
N5 C14 1.340(7) .
N5 C15 1.483(7) .
C10 C13 1.381(6) .
C11 C13 1.377(7) .
C12 C15 1.490(9) .
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
Cu1 N1 C7 C4 170.6(4)
Cu1 N1 C11 C13 -169.8(4)
N1 C11 C13 C10 -1.4(8)
C2 C6 C10 C4 -155.0(5)
C2 C6 C10 C13 24.3(7)
C2 C8 N5 C14 2.1(8)
C2 C8 N5 C15 -176.0(5)
C4 C10 C13 C11 0.0(7)
C5 C6 C10 C4 25.0(7)
C5 C6 C10 C13 -155.7(5)
C6 C2 C8 N5 -0.9(8)
C6 C5 C14 N5 -0.8(8)
C6 C10 C13 C11 -179.3(5)
C7 N1 C11 C13 1.8(8)
C7 C4 C10 C6 -179.7(5)
C7 C4 C10 C13 1.0(7)
C8 C2 C6 C5 -1.1(7)
C8 C2 C6 C10 178.9(5)
C8 N5 C14 C5 -1.3(8)
C8 N5 C15 C12 -117.1(6)
C10 C4 C7 N1 -0.6(8)
C11 N1 C7 C4 -0.7(7)
C14 C5 C6 C2 1.9(7)
C14 C5 C6 C10 -178.0(5)
C14 N5 C15 C12 64.7(8)
C15 N5 C14 C5 176.9(5)
