#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:35:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180188 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/84/7108439.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_7108439
loop_
_publ_author_name
'Gao-Chao Lv'
'Peng Wang'
'Qing Liu'
Jian
Fan
'Kai Chen'
'Wei-Yin Sun'
_publ_section_title
;
 Unprecedented crystal dynamics: reversible cascades of
 single-crystal-to-single-crystal transformations
;
_journal_name_full               Chem.Commun.
_journal_page_first              10249
_journal_paper_doi               10.1039/c2cc35456j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C34 H59 Cu N13 O10 S3'
_chemical_formula_weight         969.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.337(13)
_cell_length_b                   38.203(16)
_cell_length_c                   7.079(3)
_cell_measurement_temperature    293(2)
_cell_volume                     8475(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.2998
_diffrn_reflns_av_sigmaI/netI    0.1674
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            18284
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.8670
_exptl_absorpt_correction_T_min  0.8097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Brucker, 2000'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
This unit cell contains around 56 methanol and 16 DMSO molecules
which have been treated as a diffuse contribution to the
overall scattering without specific
atom positions by squeeze/platon.
;
_refine_diff_density_max         3.748
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4182
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.1248
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1418P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2856
_refine_ls_wR_factor_ref         0.3027
_reflns_number_gt                2103
_reflns_number_total             4182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35456j.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'Cmcm '
_cod_database_code               7108439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.0000 0.23816(3) 0.00033(13) 0.0323(4) Uani 1 2 d S
S1 S 0.0000 0.31880(16) -0.2500 0.217(5) Uani 1 4 d SU
S2 S 0.0000 0.15793(13) 0.2500 0.158(3) Uani 1 4 d SU
O1 O 0.0000 0.2818(4) -0.2500 0.213(5) Uani 1 4 d SU
O2 O 0.0000 0.1965(3) 0.2500 0.156(3) Uani 1 4 d SU
N1 N 0.2407(3) 0.38296(18) 0.2500 0.047(2) Uani 1 2 d S
N2 N 0.07694(18) 0.28138(13) 0.0922(7) 0.0399(14) Uani 1 1 d .
N3 N 0.04445(17) 0.26216(13) 0.1570(6) 0.0341(13) Uani 1 1 d .
N4 N 0.1922(5) 0.5488(3) 0.2500 0.146(5) Uani 1 2 d SDU
N5 N 0.2043(5) 0.5836(3) 0.2500 0.154(5) Uani 1 2 d SDU
N6 N 0.2484(5) 0.5870(3) 0.2500 0.158(5) Uani 1 2 d SDU
N7 N 0.2638(4) 0.5531(3) 0.2500 0.150(5) Uani 1 2 d SDU
C1 C 0.2367(4) 0.4196(2) 0.2500 0.041(2) Uani 1 2 d S
C2 C 0.1977(4) 0.4358(2) 0.2500 0.050(3) Uani 1 2 d S
H2 H 0.1727 0.4226 0.2500 0.060 Uiso 1 2 calc SR
C3 C 0.1961(5) 0.4720(3) 0.2500 0.073(4) Uani 1 2 d S
H3 H 0.1695 0.4827 0.2500 0.087 Uiso 1 2 calc SR
C4 C 0.2317(4) 0.4930(2) 0.2500 0.047(3) Uani 1 2 d S
C5 C 0.2702(5) 0.4772(3) 0.2500 0.079(4) Uani 1 2 d S
H5 H 0.2950 0.4906 0.2500 0.095 Uiso 1 2 calc SR
C6 C 0.2732(5) 0.4400(3) 0.2500 0.065(4) Uani 1 2 d S
H6 H 0.2999 0.4294 0.2500 0.077 Uiso 1 2 calc SR
C7 C 0.2298(5) 0.5296(3) 0.2500 0.135(5) Uani 1 2 d SDU
C8 C 0.2042(3) 0.3612(2) 0.2500 0.046(3) Uani 1 2 d S
C9 C 0.1855(3) 0.3503(2) 0.0807(12) 0.075(3) Uani 1 1 d .
H9 H 0.1961 0.3584 -0.0341 0.090 Uiso 1 1 calc R
C10 C 0.1517(3) 0.3279(2) 0.0841(10) 0.068(3) Uani 1 1 d .
H10 H 0.1400 0.3203 -0.0294 0.082 Uiso 1 1 calc R
C11 C 0.1347(3) 0.3164(2) 0.2500 0.037(2) Uani 1 2 d S
C12 C 0.0957(3) 0.2930(2) 0.2500 0.033(2) Uani 1 2 d S
C13 C 0.2814(3) 0.3660(2) 0.2500 0.046(3) Uani 1 2 d S
C18 C 0.0477(6) 0.1404(4) 0.2500 0.161(4) Uani 1 2 d SU
C19 C 0.0000 0.3399(4) -0.045(4) 0.221(5) Uani 1 2 d SU
N8 N 0.45478(16) 0.28519(13) 0.3435(6) 0.0334(12) Uani 1 1 d .
N9 N 0.42046(17) 0.30078(13) 0.4052(7) 0.0367(13) Uani 1 1 d .
C14 C 0.3010(3) 0.3575(2) 0.4165(12) 0.079(3) Uani 1 1 d .
H14 H 0.2886 0.3638 0.5309 0.094 Uiso 1 1 calc R
C15 C 0.3392(3) 0.3395(3) 0.4137(11) 0.082(3) Uani 1 1 d .
H15A H 0.3517 0.3333 0.5280 0.099 Uiso 1 1 calc R
C16 C 0.3593(3) 0.3306(2) 0.2500 0.042(3) Uani 1 2 d S
C17 C 0.3992(3) 0.3113(2) 0.2500 0.0285(19) Uani 1 2 d S
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'
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'
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
N3 Cu1 N3 88.1(3) 11 .
N3 Cu1 N8 91.07(19) 11 16_455
N3 Cu1 N8 179.0(2) . 16_455
N3 Cu1 N8 179.0(2) 11 6_554
N3 Cu1 N8 91.07(19) . 6_554
N8 Cu1 N8 89.7(3) 16_455 6_554
N3 Cu1 O2 84.0(2) 11 .
N3 Cu1 O2 84.0(2) . .
N8 Cu1 O2 96.5(2) 16_455 .
N8 Cu1 O2 96.5(2) 6_554 .
N3 Cu1 O1 95.1(2) 11 .
N3 Cu1 O1 95.1(2) . .
N8 Cu1 O1 84.4(2) 16_455 .
N8 Cu1 O1 84.4(2) 6_554 .
O2 Cu1 O1 178.7(3) . .
O1 S1 C19 119.1(7) . 10
O1 S1 C19 119.1(7) . .
C19 S1 C19 121.9(13) 10 .
O2 S2 C18 114.2(6) . .
O2 S2 C18 114.2(6) . 11
C18 S2 C18 131.7(11) . 11
S1 O1 Cu1 133.3(2) . 10
S1 O1 Cu1 133.3(2) . .
Cu1 O1 Cu1 93.5(5) 10 .
S2 O2 Cu1 132.0(2) . 10_556
S2 O2 Cu1 132.0(2) . .
Cu1 O2 Cu1 96.0(4) 10_556 .
C1 N1 C8 120.9(9) . .
C1 N1 C13 122.0(9) . .
C8 N1 C13 117.1(7) . .
N3 N2 C12 103.3(5) . .
N3 N3 N2 110.1(3) 10_556 .
N3 N3 Cu1 123.63(14) 10_556 .
N2 N3 Cu1 126.2(3) . .
N5 N4 C7 106.0(12) . .
N4 N5 N6 111.2(10) . .
N7 N6 N5 105.1(9) . .
N6 N7 C7 109.6(9) . .
C2 C1 C6 119.0(10) . .
C2 C1 N1 121.8(9) . .
C6 C1 N1 119.2(11) . .
C1 C2 C3 118.7(11) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C4 C3 C2 123.7(13) . .
C4 C3 H3 118.2 . .
C2 C3 H3 118.2 . .
C5 C4 C3 117.8(10) . .
C5 C4 C7 118.9(12) . .
C3 C4 C7 123.3(13) . .
C4 C5 C6 120.2(12) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C1 C6 C5 120.6(13) . .
C1 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
N4 C7 N7 108.0(11) . .
N4 C7 C4 124.2(12) . .
N7 C7 C4 127.7(13) . .
C9 C8 C9 118.2(9) . 10_556
C9 C8 N1 120.9(5) . .
C9 C8 N1 120.9(5) 10_556 .
C10 C9 C8 119.8(7) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C10 C11 121.5(7) . .
C9 C10 H10 119.2 . .
C11 C10 H10 119.2 . .
C10 C11 C10 119.0(9) 10_556 .
C10 C11 C12 120.5(5) 10_556 .
C10 C11 C12 120.5(5) . .
N2 C12 N2 113.2(8) . 10_556
N2 C12 C11 123.4(4) . .
N2 C12 C11 123.4(4) 10_556 .
C14 C13 C14 119.1(11) . 10_556
C14 C13 N1 120.4(5) . .
C14 C13 N1 120.4(5) 10_556 .
N9 N8 N8 109.6(3) . 10_556
N9 N8 Cu1 126.8(3) . 6
N8 N8 Cu1 123.54(13) 10_556 6
N8 N9 C17 105.7(5) . .
C13 C14 C15 119.6(8) . .
C13 C14 H14 120.2 . .
C15 C14 H14 120.2 . .
C16 C15 C14 122.5(8) . .
C16 C15 H15A 118.7 . .
C14 C15 H15A 118.7 . .
C15 C16 C15 116.5(10) 10_556 .
C15 C16 C17 121.7(5) 10_556 .
C15 C16 C17 121.7(5) . .
N9 C17 N9 109.5(7) 10_556 .
N9 C17 C16 125.3(4) 10_556 .
N9 C17 C16 125.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 2.003(5) 11
Cu1 N3 2.003(5) .
Cu1 N8 2.009(5) 16_455
Cu1 N8 2.009(5) 6_554
Cu1 O2 2.378(8) .
Cu1 O1 2.433(9) .
S1 O1 1.413(15) .
S1 C19 1.66(2) 10
S1 C19 1.66(2) .
S2 O2 1.474(13) .
S2 C18 1.639(19) .
S2 C18 1.639(19) 11
O1 Cu1 2.433(9) 10
O2 Cu1 2.378(8) 10_556
N1 C1 1.407(11) .
N1 C8 1.415(12) .
N1 C13 1.431(13) .
N2 N3 1.336(7) .
N2 C12 1.338(7) .
N3 N3 1.316(9) 10_556
N4 N5 1.383(9) .
N4 C7 1.387(9) .
N5 N6 1.388(9) .
N6 N7 1.384(9) .
N7 C7 1.392(9) .
C1 C2 1.371(14) .
C1 C6 1.382(15) .
C2 C3 1.385(14) .
C2 H2 0.9300 .
C3 C4 1.373(17) .
C3 H3 0.9300 .
C4 C5 1.350(18) .
C4 C7 1.401(14) .
C5 C6 1.422(15) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C8 C9 1.397(9) .
C8 C9 1.397(9) 10_556
C9 C10 1.361(9) .
C9 H9 0.9300 .
C10 C11 1.363(8) .
C10 H10 0.9300 .
C11 C10 1.363(8) 10_556
C11 C12 1.514(12) .
C12 N2 1.338(7) 10_556
C13 C14 1.367(9) .
C13 C14 1.367(9) 10_556
N8 N9 1.305(6) .
N8 N8 1.324(8) 10_556
N8 Cu1 2.009(5) 6
N9 C17 1.345(7) .
C14 C15 1.382(11) .
C14 H14 0.9300 .
C15 C16 1.363(9) .
C15 H15A 0.9300 .
C16 C15 1.363(9) 10_556
C16 C17 1.452(12) .
C17 N9 1.345(7) 10_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.015 824 349
2 0.000 0.500 0.230 757 319
3 0.250 0.250 0.703 283 90
4 0.250 0.750 0.221 283 89
5 0.500 0.500 0.705 824 349
6 0.500 0.000 0.027 757 319
7 0.750 0.250 0.221 283 89
8 0.750 0.750 0.703 283 90
