#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:35:16 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229627 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/59/7045920.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_7045920
loop_
_publ_author_name
'Naskar, Sourenjit'
'Jana, Barun'
'Ghosh, Pradyut'
_publ_section_title
;
 Anion-dependent thermo-responsive supramolecular superstructures of
 Cu(ii) macrocycles.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5734
_journal_page_last               5742
_journal_paper_doi               10.1039/c8dt00683k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C31 H37 Cl2 Cu N13 O15'
_chemical_formula_weight         966.18
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           Triclinic'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-11-26 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.835(2)
_cell_angle_beta                 101.818(2)
_cell_angle_gamma                97.050(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5428(11)
_cell_length_b                   14.4035(16)
_cell_length_c                   16.5243(18)
_cell_measurement_reflns_used    4338
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.21
_cell_measurement_theta_min      2.22
_cell_volume                     2099.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'mercury v3.6'
_computing_publication_material  'ORTEP 3v2'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19917
_diffrn_reflns_theta_full        22.31
_diffrn_reflns_theta_max         22.31
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                4179
_reflns_number_total             5338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00683k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045918--7045923.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7045920
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.27997(5) 0.80260(3) 0.31884(3) 0.0334(2) Uani 1 1 d .
Cl2 Cl 0.11971(14) 0.31438(9) 0.65772(8) 0.0535(4) Uani 1 1 d .
Cl3 Cl 0.24865(15) 0.14213(10) 0.14998(8) 0.0596(4) Uani 1 1 d .
N7 N 0.3769(3) 0.8195(2) 0.4438(2) 0.0309(8) Uani 1 1 d .
N6 N 0.1707(4) 0.9979(2) 0.3468(2) 0.0349(8) Uani 1 1 d .
N11 N 0.1804(4) 0.5041(2) 0.2502(2) 0.0371(9) Uani 1 1 d .
N4 N 0.1782(4) 1.0714(2) 0.4174(2) 0.0320(8) Uani 1 1 d .
N5 N 0.2393(3) 0.9340(2) 0.3744(2) 0.0317(8) Uani 1 1 d .
N3 N -0.1089(4) 1.2227(3) 0.4243(2) 0.0412(9) Uani 1 1 d .
H3 H -0.0947 1.2722 0.4701 0.049 Uiso 1 1 calc R
N10 N 0.2673(4) 0.5851(2) 0.3067(2) 0.0407(9) Uani 1 1 d .
N8 N 0.1612(4) 0.7837(3) 0.1977(2) 0.0372(9) Uani 1 1 d .
N1 N -0.2194(4) 1.3856(3) 0.4338(2) 0.0363(9) Uani 1 1 d .
N2 N -0.1258(4) 1.5307(3) 0.5864(3) 0.0447(10) Uani 1 1 d .
H2 H -0.0850 1.4806 0.5724 0.054 Uiso 1 1 calc R
N9 N 0.2391(4) 0.6566(2) 0.2744(2) 0.0356(9) Uani 1 1 d .
O2 O -0.2215(4) 1.1573(3) 0.2829(2) 0.0605(9) Uani 1 1 d .
O3 O 0.4907(3) 0.8375(2) 0.2877(2) 0.0488(8) Uani 1 1 d .
O1 O -0.2936(4) 1.6147(3) 0.5420(2) 0.0657(10) Uani 1 1 d .
C17 C 0.4509(5) 0.7577(3) 0.4754(3) 0.0383(11) Uani 1 1 d .
H17 H 0.4588 0.6992 0.4368 0.046 Uiso 1 1 calc R
C16 C 0.5146(5) 0.7772(3) 0.5619(3) 0.0393(11) Uani 1 1 d .
H16 H 0.5647 0.7325 0.5809 0.047 Uiso 1 1 calc R
C7 C -0.2601(5) 1.3150(3) 0.3579(3) 0.0378(11) Uani 1 1 d .
C10 C 0.1081(5) 1.1545(3) 0.4090(3) 0.0379(11) Uani 1 1 d .
H10A H 0.0955 1.1581 0.3503 0.045 Uiso 1 1 calc R
H10B H 0.1693 1.2154 0.4485 0.045 Uiso 1 1 calc R
C11 C 0.2486(4) 1.0559(3) 0.4897(3) 0.0316(10) Uani 1 1 d .
H11 H 0.2665 1.0965 0.5466 0.038 Uiso 1 1 calc R
C3 C -0.2803(5) 1.4655(3) 0.4414(3) 0.0396(11) Uani 1 1 d .
C14 C 0.4308(4) 0.9279(3) 0.5897(3) 0.0344(10) Uani 1 1 d .
H14 H 0.4237 0.9870 0.6278 0.041 Uiso 1 1 calc R
C12 C 0.2885(4) 0.9666(3) 0.4614(3) 0.0315(10) Uani 1 1 d .
C24 C 0.0979(5) 0.5219(3) 0.1822(3) 0.0422(11) Uani 1 1 d .
H24 H 0.0293 0.4770 0.1351 0.051 Uiso 1 1 calc R
C2 C -0.2348(5) 1.5433(3) 0.5272(3) 0.0442(12) Uani 1 1 d .
C15 C 0.5044(5) 0.8624(3) 0.6203(3) 0.0377(11) Uani 1 1 d .
H15 H 0.5461 0.8762 0.6793 0.045 Uiso 1 1 calc R
C23 C 0.1372(5) 0.6206(3) 0.1975(3) 0.0359(10) Uani 1 1 d .
C13 C 0.3681(4) 0.9044(3) 0.5018(3) 0.0271(9) Uani 1 1 d .
C8 C -0.1951(5) 1.2242(3) 0.3508(3) 0.0389(11) Uani 1 1 d .
C18 C 0.1361(5) 0.8551(3) 0.1610(3) 0.0483(12) Uani 1 1 d .
H18 H 0.1812 0.9198 0.1917 0.058 Uiso 1 1 calc R
C6 C -0.3606(5) 1.3212(4) 0.2871(3) 0.0498(13) Uani 1 1 d .
H6 H -0.3863 1.2707 0.2347 0.060 Uiso 1 1 calc R
C25 C 0.1768(5) 0.4104(3) 0.2705(3) 0.0449(12) Uani 1 1 d .
H25A H 0.2741 0.4069 0.2999 0.054 Uiso 1 1 calc R
H25B H 0.1455 0.3561 0.2170 0.054 Uiso 1 1 calc R
C22 C 0.0958(5) 0.6906(3) 0.1521(3) 0.0371(11) Uani 1 1 d .
C19 C 0.0467(6) 0.8352(4) 0.0802(3) 0.0526(13) Uani 1 1 d .
H19 H 0.0325 0.8853 0.0557 0.063 Uiso 1 1 calc R
C9 C -0.0386(5) 1.1415(3) 0.4300(3) 0.0423(11) Uani 1 1 d .
H9A H -0.0999 1.0811 0.3898 0.051 Uiso 1 1 calc R
H9B H -0.0256 1.1362 0.4882 0.051 Uiso 1 1 calc R
C4 C -0.3810(5) 1.4769(4) 0.3746(4) 0.0557(14) Uani 1 1 d .
H4 H -0.4212 1.5334 0.3823 0.067 Uiso 1 1 calc R
C1 C -0.0752(5) 1.5987(3) 0.6730(3) 0.0465(12) Uani 1 1 d .
H1A H -0.0622 1.6652 0.6693 0.056 Uiso 1 1 calc R
H1B H 0.0191 1.5879 0.6999 0.056 Uiso 1 1 calc R
C5 C -0.4220(6) 1.4043(4) 0.2963(4) 0.0609(15) Uani 1 1 d .
H5 H -0.4900 1.4108 0.2501 0.073 Uiso 1 1 calc R
C21 C 0.0038(5) 0.6661(4) 0.0714(3) 0.0495(12) Uani 1 1 d .
H21 H -0.0402 0.6010 0.0414 0.059 Uiso 1 1 calc R
C20 C -0.0225(6) 0.7396(4) 0.0354(3) 0.0583(14) Uani 1 1 d .
H20 H -0.0867 0.7250 -0.0189 0.070 Uiso 1 1 calc R
O4 O 0.0500(5) 0.3657(3) 0.6058(3) 0.1002(15) Uani 1 1 d .
O6 O 0.2315(4) 0.2783(3) 0.6237(3) 0.0850(13) Uani 1 1 d .
O5 O 0.1769(6) 0.3772(4) 0.7424(3) 0.1155(18) Uani 1 1 d .
O7 O 0.0183(6) 0.2347(3) 0.6588(4) 0.1140(18) Uani 1 1 d .
O11 O 0.3472(6) 0.0781(4) 0.1572(3) 0.1110(18) Uani 1 1 d .
O8 O 0.1156(6) 0.0883(5) 0.0961(4) 0.151(2) Uani 1 1 d .
O9 O 0.2974(7) 0.2108(5) 0.1120(4) 0.151(2) Uani 1 1 d .
O10 O 0.2372(7) 0.1926(4) 0.2340(3) 0.1211(19) Uani 1 1 d .
N12 N 0.2634(5) 0.8395(3) 0.9298(3) 0.0664(13) Uani 1 1 d .
C26 C 0.2729(9) 0.9383(5) 0.9240(5) 0.101(2) Uani 1 1 d .
H26A H 0.1873 0.9419 0.8835 0.152 Uiso 1 1 calc R
H26B H 0.3577 0.9554 0.9045 0.152 Uiso 1 1 calc R
H26C H 0.2798 0.9834 0.9801 0.152 Uiso 1 1 calc R
C27 C 0.3784(8) 0.8197(6) 0.9895(5) 0.114(3) Uani 1 1 d .
H27A H 0.3426 0.7635 1.0052 0.170 Uiso 1 1 calc R
H27B H 0.4126 0.8757 1.0407 0.170 Uiso 1 1 calc R
H27C H 0.4572 0.8066 0.9628 0.170 Uiso 1 1 calc R
C28 C 0.1574(6) 0.7677(5) 0.8772(3) 0.0659(15) Uani 1 1 d .
H28 H 0.0867 0.7840 0.8384 0.079 Uiso 1 1 calc R
O12 O 0.1443(5) 0.6817(3) 0.8752(3) 0.0825(12) Uani 1 1 d .
C29 C 0.5202(6) 0.7816(4) 0.2248(3) 0.0532(13) Uani 1 1 d .
H29 H 0.4595 0.7203 0.1989 0.064 Uiso 1 1 calc R
N13 N 0.6288(5) 0.8006(3) 0.1915(3) 0.0577(12) Uani 1 1 d .
C30 C 0.6562(8) 0.7272(5) 0.1180(4) 0.095(2) Uani 1 1 d .
H30A H 0.7481 0.7088 0.1360 0.142 Uiso 1 1 calc R
H30B H 0.6584 0.7545 0.0713 0.142 Uiso 1 1 calc R
H30C H 0.5798 0.6701 0.0986 0.142 Uiso 1 1 calc R
C31 C 0.7314(8) 0.8935(5) 0.2319(5) 0.107(3) Uani 1 1 d .
H31A H 0.6949 0.9432 0.2096 0.161 Uiso 1 1 calc R
H31B H 0.8239 0.8860 0.2192 0.161 Uiso 1 1 calc R
H31C H 0.7433 0.9127 0.2937 0.161 Uiso 1 1 calc R
O13 O 0.3170(6) 0.5457(4) 0.8850(4) 0.1187(17) Uani 1 1 d .
O17 O 0.3828(9) 0.3990(7) 0.0961(5) 0.211(4) Uani 1 1 d .
O18 O 0.2983(13) 0.5370(7) 0.0465(6) 0.256(6) 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'
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_3
N9 Cu1 N5 155.31(14) .
N9 Cu1 N7 98.65(14) .
N5 Cu1 N7 80.55(13) .
N9 Cu1 N8 80.71(14) .
N5 Cu1 N8 97.28(14) .
N7 Cu1 N8 173.43(13) .
N9 Cu1 O3 101.17(13) .
N5 Cu1 O3 103.51(12) .
N7 Cu1 O3 92.58(13) .
N8 Cu1 O3 93.96(13) .
O6 Cl2 O5 109.9(3) .
O6 Cl2 O4 109.4(3) .
O5 Cl2 O4 109.6(3) .
O6 Cl2 O7 109.1(3) .
O5 Cl2 O7 109.2(3) .
O4 Cl2 O7 109.7(3) .
O8 Cl3 O9 107.2(4) .
O8 Cl3 O11 109.0(4) .
O9 Cl3 O11 110.7(4) .
O8 Cl3 O10 112.4(4) .
O9 Cl3 O10 108.6(4) .
O11 Cl3 O10 108.9(3) .
C13 N7 C17 117.1(4) .
C13 N7 Cu1 115.2(3) .
C17 N7 Cu1 127.7(3) .
N5 N6 N4 105.8(3) .
N10 N11 C24 112.5(3) .
N10 N11 C25 119.3(4) .
C24 N11 C25 128.1(4) .
N6 N4 C11 112.1(3) .
N6 N4 C10 119.5(3) .
C11 N4 C10 128.3(4) .
N6 N5 C12 110.2(3) .
N6 N5 Cu1 135.3(3) .
C12 N5 Cu1 114.5(3) .
C8 N3 C9 122.4(4) .
N9 N10 N11 105.4(3) .
C22 N8 C18 118.2(4) .
C22 N8 Cu1 115.3(3) .
C18 N8 Cu1 126.5(3) .
C7 N1 C3 117.8(4) .
C2 N2 C1 121.7(4) .
N10 N9 C23 110.3(3) .
N10 N9 Cu1 135.7(3) .
C23 N9 Cu1 112.8(3) .
C29 O3 Cu1 120.1(3) .
N7 C17 C16 122.9(4) .
C15 C16 C17 119.9(4) .
N1 C7 C6 122.9(4) .
N1 C7 C8 117.5(4) .
C6 C7 C8 119.5(4) .
N4 C10 C9 109.6(3) .
N4 C11 C12 104.6(4) .
N1 C3 C4 122.8(5) .
N1 C3 C2 117.1(4) .
C4 C3 C2 120.1(4) .
C15 C14 C13 119.2(4) .
N5 C12 C11 107.3(4) .
N5 C12 C13 116.8(3) .
C11 C12 C13 135.9(4) .
N11 C24 C23 104.5(4) .
O1 C2 N2 122.4(5) .
O1 C2 C3 121.4(5) .
N2 C2 C3 116.3(4) .
C16 C15 C14 118.6(4) .
N9 C23 C24 107.4(4) .
N9 C23 C22 117.1(4) .
C24 C23 C22 135.5(4) .
N7 C13 C14 122.4(4) .
N7 C13 C12 113.0(3) .
C14 C13 C12 124.6(4) .
O2 C8 N3 123.3(4) .
O2 C8 C7 122.2(4) .
N3 C8 C7 114.6(4) .
N8 C18 C19 121.9(5) .
C5 C6 C7 118.3(5) .
N11 C25 C1 111.1(4) 2_576
N8 C22 C21 122.6(4) .
N8 C22 C23 112.6(4) .
C21 C22 C23 124.8(4) .
C18 C19 C20 119.0(5) .
N3 C9 C10 111.1(3) .
C5 C4 C3 119.3(5) .
N2 C1 C25 113.4(4) 2_576
C4 C5 C6 118.9(5) .
C22 C21 C20 118.6(5) .
C21 C20 C19 119.7(5) .
C28 N12 C26 121.1(6) .
C28 N12 C27 120.5(6) .
C26 N12 C27 118.2(5) .
O12 C28 N12 125.5(6) .
O3 C29 N13 126.0(5) .
C29 N13 C31 119.4(5) .
C29 N13 C30 121.3(5) .
C31 N13 C30 119.1(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N9 1.988(3) .
Cu1 N5 1.988(3) .
Cu1 N7 2.017(3) .
Cu1 N8 2.015(4) .
Cu1 O3 2.209(3) .
Cl2 O6 1.395(4) .
Cl2 O5 1.396(4) .
Cl2 O4 1.399(4) .
Cl2 O7 1.414(4) .
Cl3 O8 1.387(5) .
Cl3 O9 1.391(5) .
Cl3 O11 1.405(4) .
Cl3 O10 1.414(5) .
N7 C13 1.355(5) .
N7 C17 1.349(5) .
N6 N5 1.318(4) .
N6 N4 1.326(5) .
N11 N10 1.332(5) .
N11 C24 1.338(6) .
N11 C25 1.475(5) .
N4 C11 1.336(5) .
N4 C10 1.466(5) .
N5 C12 1.344(5) .
N3 C8 1.327(6) .
N3 C9 1.433(5) .
N10 N9 1.314(5) .
N8 C22 1.344(5) .
N8 C18 1.352(6) .
N1 C7 1.329(6) .
N1 C3 1.338(5) .
N2 C2 1.342(6) .
N2 C1 1.440(6) .
N9 C23 1.356(5) .
O2 C8 1.219(5) .
O3 C29 1.235(5) .
O1 C2 1.221(5) .
C17 C16 1.368(6) .
C16 C15 1.367(6) .
C7 C6 1.384(6) .
C7 C8 1.501(6) .
C10 C9 1.512(6) .
C11 C12 1.371(6) .
C3 C4 1.368(7) .
C3 C2 1.489(7) .
C14 C15 1.384(6) .
C14 C13 1.380(6) .
C12 C13 1.454(6) .
C24 C23 1.365(6) .
C23 C22 1.457(6) .
C18 C19 1.362(7) .
C6 C5 1.381(7) .
C25 C1 1.495(6) 2_576
C22 C21 1.365(6) .
C19 C20 1.378(7) .
C4 C5 1.369(7) .
C1 C25 1.495(6) 2_576
C21 C20 1.373(7) .
N12 C28 1.320(7) .
N12 C26 1.445(8) .
N12 C27 1.431(8) .
C28 O12 1.220(7) .
C29 N13 1.303(6) .
N13 C31 1.456(8) .
N13 C30 1.470(7) .
