#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:35:16 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180188 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/84/7108440.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_7108440
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            'C30 H43 Cu N13 O6 S3'
_chemical_formula_weight         841.49
_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                   31.552(6)
_cell_length_b                   37.319(7)
_cell_length_c                   7.1146(14)
_cell_measurement_temperature    293(2)
_cell_volume                     8377(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16379
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.8685
_exptl_absorpt_correction_T_min  0.8117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_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 16 methanol and 24 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         1.315
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1697P)²+1.5779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2241
_reflns_number_gt                2932
_reflns_number_total             4127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35456j.txt
_cod_data_source_block           3
_cod_original_cell_volume        8378(3)
_cod_original_sg_symbol_H-M      'Cmcm '
_cod_database_code               7108440
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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 0.0000 0.256125(16) 0.00000(5) 0.0388(3) Uani 1 2 d S
C1 C 0.2634(4) 0.5334(2) 0.2500 0.117(3) Uani 1 2 d S
C2 C 0.2607(3) 0.49458(16) 0.2500 0.086(2) Uani 1 2 d S
C3 C 0.2227(3) 0.47699(19) 0.2500 0.098(2) Uani 1 2 d S
H3A H 0.1977 0.4903 0.2500 0.118 Uiso 1 2 calc SR
C4 C 0.2963(3) 0.47409(19) 0.2500 0.095(2) Uani 1 2 d S
H4A H 0.3226 0.4853 0.2500 0.114 Uiso 1 2 calc SR
C5 C 0.2203(2) 0.44001(16) 0.2500 0.0811(18) Uani 1 2 d S
H5A H 0.1940 0.4288 0.2500 0.097 Uiso 1 2 calc SR
C6 C 0.29453(19) 0.43690(16) 0.2500 0.0790(17) Uani 1 2 d S
H6A H 0.3196 0.4238 0.2500 0.095 Uiso 1 2 calc SR
C7 C 0.25750(16) 0.41946(15) 0.2500 0.0639(14) Uani 1 2 d S
C8 C 0.21520(14) 0.36411(14) 0.2500 0.0657(14) Uani 1 2 d S
C9 C 0.19655(15) 0.35447(17) 0.0931(8) 0.123(2) Uani 1 1 d .
H9A H 0.2079 0.3622 -0.0205 0.147 Uiso 1 1 calc R
C10 C 0.16007(14) 0.33293(16) 0.0906(7) 0.1159(19) Uani 1 1 d .
H10 H 0.1504 0.3232 -0.0218 0.139 Uiso 1 1 calc R
C11 C 0.13953(13) 0.32658(13) 0.2500 0.0551(11) Uani 1 2 d S
C12 C 0.09968(12) 0.30614(12) 0.2500 0.0455(10) Uani 1 2 d S
C13 C 0.29234(13) 0.36103(14) 0.2500 0.0640(14) Uani 1 2 d S
C14 C 0.30894(15) 0.34984(15) 0.0900(8) 0.1129(18) Uani 1 1 d .
H14 H 0.2966 0.3566 -0.0234 0.135 Uiso 1 1 calc R
C15 C 0.34519(14) 0.32770(15) 0.0898(7) 0.1081(17) Uani 1 1 d .
H15 H 0.3560 0.3194 -0.0237 0.130 Uiso 1 1 calc R
C16 C 0.40230(12) 0.29611(12) 0.2500 0.0472(10) Uani 1 2 d S
C17 C 0.36408(12) 0.31854(13) 0.2500 0.0562(12) Uani 1 2 d S
C18 C 0.0000 0.3387(2) -0.2500 0.130(4) Uani 1 4 d S
C19 C 0.0000 0.17488(19) 0.2500 0.146(5) Uani 1 4 d S
N1 N 0.2254(4) 0.5551(2) 0.2500 0.168(5) Uani 1 2 d S
N2 N 0.2452(6) 0.5856(5) 0.2500 0.177(7) Uani 1 2 d S
N3 N 0.2925(4) 0.5539(2) 0.2500 0.162(4) Uani 1 2 d S
N4 N 0.2795(6) 0.5878(5) 0.2500 0.213(10) Uani 1 2 d S
N5 N 0.25533(11) 0.38253(12) 0.2500 0.0711(14) Uani 1 2 d S
N6 N 0.04470(6) 0.27952(7) 0.1577(3) 0.0424(6) Uani 1 1 d .
N7 N 0.07898(7) 0.29608(7) 0.0954(3) 0.0497(7) Uani 1 1 d .
N8 N 0.45540(7) 0.26748(7) 0.1581(3) 0.0432(6) Uani 1 1 d .
N9 N 0.42228(7) 0.28532(7) 0.0949(4) 0.0499(7) Uani 1 1 d .
O1A O 0.0000 0.30008(11) -0.2500 0.0569(11) Uani 1 4 d S
O2A O 0.0000 0.21200(12) 0.2500 0.0631(12) Uani 1 4 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'
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'
Cu Cu 0.3201 1.2651 '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
N6 Cu1 N6 89.55(12) . 12
N6 Cu1 N8 179.75(10) . 8_455
N6 Cu1 N8 90.66(9) 12 8_455
N6 Cu1 N8 90.66(9) . 13
N6 Cu1 N8 179.75(10) 12 13
N8 Cu1 N8 89.13(12) 8_455 13
N6 Cu1 O1A 96.67(9) . .
N6 Cu1 O1A 96.67(9) 12 .
N8 Cu1 O1A 83.43(9) 8_455 .
N8 Cu1 O1A 83.43(9) 13 .
N6 Cu1 O2A 83.41(9) . .
N6 Cu1 O2A 83.41(9) 12 .
N8 Cu1 O2A 96.49(9) 8_455 .
N8 Cu1 O2A 96.49(9) 13 .
O1A Cu1 O2A 179.89(11) . .
N3 C1 N1 106.2(9) . .
N3 C1 C2 133.1(13) . .
N1 C1 C2 120.8(11) . .
C4 C2 C3 117.1(6) . .
C4 C2 C1 120.9(9) . .
C3 C2 C1 122.0(9) . .
C2 C3 C5 121.8(7) . .
C2 C3 H3A 119.1 . .
C5 C3 H3A 119.1 . .
C2 C4 C6 121.9(6) . .
C2 C4 H4A 119.0 . .
C6 C4 H4A 119.0 . .
C3 C5 C7 120.0(6) . .
C3 C5 H5A 120.0 . .
C7 C5 H5A 120.0 . .
C7 C6 C4 121.4(6) . .
C7 C6 H6A 119.3 . .
C4 C6 H6A 119.3 . .
C6 C7 N5 122.0(5) . .
C6 C7 C5 117.7(5) . .
N5 C7 C5 120.3(5) . .
C9 C8 C9 116.6(5) . 10_556
C9 C8 N5 121.7(3) . .
C9 C8 N5 121.7(3) 10_556 .
C8 C9 C10 122.4(5) . .
C8 C9 H9A 118.8 . .
C10 C9 H9A 118.8 . .
C11 C10 C9 119.4(5) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
C10 C11 C10 117.3(5) 10_556 .
C10 C11 C12 120.7(2) 10_556 .
C10 C11 C12 120.7(2) . .
N7 C12 N7 111.2(3) . 10_556
N7 C12 C11 124.40(17) . .
N7 C12 C11 124.40(17) 10_556 .
C14 C13 C14 119.0(5) 10_556 .
C14 C13 N5 120.4(2) 10_556 .
C14 C13 N5 120.4(2) . .
C13 C14 C15 120.5(4) . .
C13 C14 H14 119.8 . .
C15 C14 H14 119.8 . .
C17 C15 C14 120.8(4) . .
C17 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
N9 C16 N9 111.7(3) 10_556 .
N9 C16 C17 124.10(17) 10_556 .
N9 C16 C17 124.10(17) . .
C15 C17 C15 117.8(5) . 10_556
C15 C17 C16 121.0(2) . .
C15 C17 C16 121.0(2) 10_556 .
N2 N1 C1 95.4(13) . .
N4 N2 N1 123(3) . .
C1 N3 N4 111.7(16) . .
N2 N4 N3 104(2) . .
C7 N5 C13 121.7(4) . .
C7 N5 C8 121.3(4) . .
C13 N5 C8 117.0(4) . .
N6 N6 N7 109.57(14) 10_556 .
N6 N6 Cu1 124.07(6) 10_556 .
N7 N6 Cu1 126.33(17) . .
N6 N7 C12 104.8(2) . .
N8 N8 N9 109.94(14) 10_556 .
N8 N8 Cu1 124.12(6) 10_556 13
N9 N8 Cu1 125.94(18) . 13
N8 N9 C16 104.2(2) . .
C18 O1A Cu1 132.69(7) . 10
C18 O1A Cu1 132.69(7) . .
Cu1 O1A Cu1 94.63(15) 10 .
C19 O2A Cu1 132.80(8) . .
C19 O2A Cu1 132.80(8) . 10_556
Cu1 O2A Cu1 94.41(16) . 10_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N6 2.002(2) .
Cu1 N6 2.002(2) 12
Cu1 N8 2.006(2) 8_455
Cu1 N8 2.006(2) 13
Cu1 O1A 2.420(3) .
Cu1 O2A 2.424(3) .
C1 N3 1.196(14) .
C1 N1 1.445(16) .
C1 C2 1.453(10) .
C2 C4 1.359(10) .
C2 C3 1.367(11) .
C3 C5 1.382(9) .
C3 H3A 0.9300 .
C4 C6 1.389(9) .
C4 H4A 0.9300 .
C5 C7 1.403(7) .
C5 H5A 0.9300 .
C6 C7 1.338(7) .
C6 H6A 0.9300 .
C7 N5 1.380(8) .
C8 C9 1.312(5) .
C8 C9 1.312(5) 10_556
C8 N5 1.441(5) .
C9 C10 1.404(5) .
C9 H9A 0.9300 .
C10 C11 1.328(5) .
C10 H10 0.9300 .
C11 C10 1.328(5) 10_556
C11 C12 1.470(5) .
C12 N7 1.333(3) .
C12 N7 1.333(3) 10_556
C13 C14 1.321(5) 10_556
C13 C14 1.321(5) .
C13 N5 1.417(6) .
C14 C15 1.411(5) .
C14 H14 0.9300 .
C15 C17 1.331(5) .
C15 H15 0.9300 .
C16 N9 1.333(3) 10_556
C16 N9 1.333(3) .
C16 C17 1.468(5) .
C17 C15 1.331(5) 10_556
C18 O1A 1.441(9) .
C19 O2A 1.385(8) .
N1 N2 1.296(19) .
N2 N4 1.09(3) .
N3 N4 1.33(2) .
N6 N6 1.314(4) 10_556
N6 N7 1.322(3) .
N8 N8 1.308(4) 10_556
N8 N9 1.318(3) .
N8 Cu1 2.006(2) 13
O1A Cu1 2.420(3) 10
O2A Cu1 2.424(3) 10_556
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_1
_geom_torsion_site_symmetry_4
N3 C1 C2 C4 0.0 . .
N1 C1 C2 C4 180.0 . .
N3 C1 C2 C3 180.0 . .
N1 C1 C2 C3 0.0 . .
C4 C2 C3 C5 0.0 . .
C1 C2 C3 C5 180.0 . .
C3 C2 C4 C6 0.0 . .
C1 C2 C4 C6 180.0 . .
C2 C3 C5 C7 0.0 . .
C2 C4 C6 C7 0.0 . .
C4 C6 C7 N5 180.0 . .
C4 C6 C7 C5 0.0 . .
C3 C5 C7 C6 0.0 . .
C3 C5 C7 N5 180.0 . .
C9 C8 C9 C10 -4.2(11) 10_556 .
N5 C8 C9 C10 172.4(5) . .
C8 C9 C10 C11 11.0(10) . .
C9 C10 C11 C10 -17.1(11) . 10_556
C9 C10 C11 C12 175.9(5) . .
C10 C11 C12 N7 -174.2(5) 10_556 .
C10 C11 C12 N7 -7.7(7) . .
C10 C11 C12 N7 7.7(7) 10_556 10_556
C10 C11 C12 N7 174.2(5) . 10_556
C14 C13 C14 C15 -3.2(11) 10_556 .
N5 C13 C14 C15 -178.4(5) . .
C13 C14 C15 C17 -2.0(9) . .
C14 C15 C17 C15 7.0(11) . 10_556
C14 C15 C17 C16 -178.8(5) . .
N9 C16 C17 C15 -178.5(5) 10_556 .
N9 C16 C17 C15 4.5(8) . .
N9 C16 C17 C15 -4.5(8) 10_556 10_556
N9 C16 C17 C15 178.5(5) . 10_556
N3 C1 N1 N2 0.0 . .
C2 C1 N1 N2 180.0 . .
C1 N1 N2 N4 0.0 . .
N1 C1 N3 N4 0.0 . .
C2 C1 N3 N4 180.0 . .
N1 N2 N4 N3 0.0 . .
C1 N3 N4 N2 0.0 . .
C6 C7 N5 C13 0.0 . .
C5 C7 N5 C13 180.0 . .
C6 C7 N5 C8 180.0 . .
C5 C7 N5 C8 0.0 . .
C14 C13 N5 C7 92.4(5) 10_556 .
C14 C13 N5 C7 -92.4(5) . .
C14 C13 N5 C8 -87.6(5) 10_556 .
C14 C13 N5 C8 87.6(5) . .
C9 C8 N5 C7 91.8(5) . .
C9 C8 N5 C7 -91.8(5) 10_556 .
C9 C8 N5 C13 -88.2(5) . .
C9 C8 N5 C13 88.2(5) 10_556 .
N6 Cu1 N6 N6 47.86(11) 12 10_556
N8 Cu1 N6 N6 -101(38) 8_455 10_556
N8 Cu1 N6 N6 -132.02(8) 13 10_556
O1A Cu1 N6 N6 144.52(7) . 10_556
O2A Cu1 N6 N6 -35.56(7) . 10_556
N6 Cu1 N6 N7 -134.49(19) 12 .
N8 Cu1 N6 N7 76(32) 8_455 .
N8 Cu1 N6 N7 45.6(2) 13 .
O1A Cu1 N6 N7 -37.8(2) . .
O2A Cu1 N6 N7 142.1(2) . .
N6 N6 N7 C12 -0.1(3) 10_556 .
Cu1 N6 N7 C12 -178.0(2) . .
N7 C12 N7 N6 0.1(5) 10_556 .
C11 C12 N7 N6 -178.2(4) . .
N8 N8 N9 C16 0.0(3) 10_556 .
Cu1 N8 N9 C16 -179.5(2) 13 .
N9 C16 N9 N8 -0.1(5) 10_556 .
C17 C16 N9 N8 177.3(4) . .
N6 Cu1 O1A C18 -45.17(6) . .
N6 Cu1 O1A C18 45.17(6) 12 .
N8 Cu1 O1A C18 135.06(6) 8_455 .
N8 Cu1 O1A C18 -135.06(6) 13 .
O2A Cu1 O1A C18 180(100) . .
N6 Cu1 O1A Cu1 134.83(6) . 10
N6 Cu1 O1A Cu1 -134.83(6) 12 10
N8 Cu1 O1A Cu1 -44.94(6) 8_455 10
N8 Cu1 O1A Cu1 44.94(6) 13 10
O2A Cu1 O1A Cu1 0(100) . 10
N6 Cu1 O2A C19 -134.84(6) . .
N6 Cu1 O2A C19 134.84(6) 12 .
N8 Cu1 O2A C19 44.93(6) 8_455 .
N8 Cu1 O2A C19 -44.93(6) 13 .
O1A Cu1 O2A C19 0(100) . .
N6 Cu1 O2A Cu1 45.16(6) . 10_556
N6 Cu1 O2A Cu1 -45.16(6) 12 10_556
N8 Cu1 O2A Cu1 -135.07(6) 8_455 10_556
N8 Cu1 O2A Cu1 135.07(6) 13 10_556
O1A Cu1 O2A Cu1 180(100) . 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 -0.015 877 192
2 0.000 0.500 0.188 912 206
3 0.250 0.250 0.213 257 90
4 0.250 0.750 0.210 257 90
5 0.500 0.000 0.004 911 206
6 0.500 0.500 0.727 877 192
7 0.750 0.250 0.211 257 90
8 0.750 0.750 0.213 257 90
