#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:47:40 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180196 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/92/7109211.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_7109211
loop_
_publ_author_name
'Hong-Xi Li'
'Wei Zhao'
'Hai-Yan Li'
'Zhong-Lin Xu'
'Wen-Xia Wang'
'Jian-Ping Lang'
_publ_section_title
;
 Cu30I16(mtpmt)12(mu10--S4)]: an unusual 30--membered copper(I) cluster
 derived from the C-S bond cleavage and its use in heterogeneous catalysis
;
_journal_name_full               Chem.Commun.
_journal_page_first              4259
_journal_paper_doi               10.1039/c2cc36736j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         '2(C24 H22 Cu I N4 S), 2(C N0.50 H1.5)'
_chemical_formula_sum            'C50 H47 Cu2 I2 N9 S2'
_chemical_formula_weight         1218.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.591(3)
_cell_length_b                   26.495(5)
_cell_length_c                   7.4948(15)
_cell_measurement_reflns_used    11916
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.0145
_cell_volume                     2683.8(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15400
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         6051
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0596
_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)+(0.0604P)²+4.3347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                4687
_reflns_number_total             6051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36736j.txt
_cod_data_source_block           t2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7109211
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.49953(3) 0.291612(15) 0.89762(5) 0.04118(14) Uani 1 1 d . . .
Cu1 Cu 0.40929(5) 0.27057(3) 0.58541(10) 0.03801(19) Uani 1 1 d . . .
S1 S 0.20557(11) 0.34593(5) 0.6509(2) 0.0380(3) Uani 1 1 d . . .
N1 N 0.3700(3) 0.33861(16) 0.4664(6) 0.0322(10) Uani 1 1 d . . .
N2 N 0.2792(4) 0.41500(17) 0.4699(6) 0.0361(10) Uani 1 1 d . . .
N3 N 0.2646(3) 0.24825(16) 0.6001(6) 0.0320(10) Uani 1 1 d . . .
N4 N 0.1037(3) 0.26599(16) 0.6823(6) 0.0311(9) Uani 1 1 d . . .
C1 C 0.2956(4) 0.3670(2) 0.5135(7) 0.0326(11) Uani 1 1 d . . .
C2 C 0.4270(4) 0.3615(2) 0.3545(8) 0.0386(13) Uani 1 1 d . A .
H2 H 0.4772 0.3426 0.3119 0.046 Uiso 1 1 calc R . .
C3 C 0.4167(4) 0.4111(2) 0.2980(8) 0.0405(13) Uani 1 1 d D . .
C4 C 0.3394(4) 0.4379(2) 0.3651(7) 0.0357(12) Uani 1 1 d . A .
C5 C 0.489(6) 0.434(4) 0.181(7) 0.059(8) Uani 0.50 1 d PD A 1
H5A H 0.5449 0.4473 0.2560 0.089 Uiso 0.50 1 calc PR A 1
H5B H 0.4574 0.4607 0.1103 0.089 Uiso 0.50 1 calc PR A 1
H5C H 0.5114 0.4085 0.1037 0.089 Uiso 0.50 1 calc PR A 1
C5A C 0.477(6) 0.428(4) 0.150(7) 0.059(8) Uani 0.50 1 d PD A 2
H5A1 H 0.5333 0.4467 0.2005 0.089 Uiso 0.50 1 calc PR A 2
H5A2 H 0.4364 0.4491 0.0672 0.089 Uiso 0.50 1 calc PR A 2
H5A3 H 0.4979 0.3990 0.0875 0.089 Uiso 0.50 1 calc PR A 2
C6 C 0.3129(5) 0.4915(2) 0.3184(8) 0.0462(6) Uani 1 1 d . . .
C7 C 0.2133(5) 0.5043(2) 0.2953(8) 0.0462(6) Uani 1 1 d . A .
H7 H 0.1658 0.4802 0.3145 0.055 Uiso 1 1 calc R . .
C8 C 0.1844(5) 0.5526(2) 0.2439(8) 0.0462(6) Uani 1 1 d . . .
H8 H 0.1174 0.5603 0.2248 0.055 Uiso 1 1 calc R A .
C9 C 0.2545(5) 0.5900(2) 0.2202(9) 0.0462(6) Uani 1 1 d D A .
C10 C 0.3542(5) 0.5774(2) 0.2515(8) 0.0462(6) Uani 1 1 d . . .
H10 H 0.4019 0.6020 0.2406 0.055 Uiso 1 1 calc R A .
C11 C 0.3835(5) 0.5285(2) 0.2988(8) 0.0462(6) Uani 1 1 d . A .
H11 H 0.4505 0.5205 0.3173 0.055 Uiso 1 1 calc R . .
C12 C 0.236(3) 0.6441(4) 0.158(2) 0.0462(6) Uani 0.48(8) 1 d PD A 1
H12A H 0.2069 0.6442 0.0362 0.069 Uiso 0.48(8) 1 calc PR A 1
H12B H 0.2979 0.6620 0.1671 0.069 Uiso 0.48(8) 1 calc PR A 1
H12C H 0.1922 0.6602 0.2331 0.069 Uiso 0.48(8) 1 calc PR A 1
C12A C 0.206(3) 0.6404(6) 0.165(2) 0.0462(6) Uani 0.52(8) 1 d PD A 2
H12D H 0.1818 0.6393 0.0402 0.069 Uiso 0.52(8) 1 calc PR A 2
H12E H 0.2543 0.6669 0.1849 0.069 Uiso 0.52(8) 1 calc PR A 2
H12F H 0.1524 0.6467 0.2352 0.069 Uiso 0.52(8) 1 calc PR A 2
C13 C 0.1927(4) 0.27915(19) 0.6400(7) 0.0302(11) Uani 1 1 d . . .
C14 C 0.2387(4) 0.19978(19) 0.5882(7) 0.0322(11) Uani 1 1 d . . .
H14 H 0.2849 0.1770 0.5528 0.039 Uiso 1 1 calc R . .
C15 C 0.1487(4) 0.1810(2) 0.6244(7) 0.0348(12) Uani 1 1 d . . .
C16 C 0.0810(4) 0.2165(2) 0.6810(7) 0.0310(11) Uani 1 1 d . . .
C17 C 0.1251(5) 0.1251(2) 0.5923(9) 0.0442(14) Uani 1 1 d . . .
H17A H 0.1733 0.1104 0.5231 0.066 Uiso 1 1 calc R . .
H17B H 0.0604 0.1218 0.5282 0.066 Uiso 1 1 calc R . .
H17C H 0.1267 0.1080 0.7055 0.066 Uiso 1 1 calc R . .
C18 C -0.0186(4) 0.20360(19) 0.7313(7) 0.0313(11) Uani 1 1 d . . .
C19 C -0.0979(4) 0.2352(2) 0.6769(7) 0.0350(12) Uani 1 1 d . . .
H19 H -0.0872 0.2645 0.6132 0.042 Uiso 1 1 calc R . .
C20 C -0.1928(4) 0.2236(2) 0.7164(8) 0.0385(13) Uani 1 1 d . . .
H20 H -0.2450 0.2449 0.6781 0.046 Uiso 1 1 calc R . .
C21 C -0.2107(4) 0.1799(2) 0.8135(7) 0.0352(12) Uani 1 1 d . . .
C22 C -0.1299(4) 0.1498(2) 0.8718(7) 0.0382(13) Uani 1 1 d . . .
H22 H -0.1395 0.1214 0.9408 0.046 Uiso 1 1 calc R . .
C23 C -0.0350(4) 0.1609(2) 0.8298(8) 0.0372(12) Uani 1 1 d . . .
H23 H 0.0175 0.1397 0.8681 0.045 Uiso 1 1 calc R . .
C24 C -0.3137(5) 0.1663(3) 0.8496(9) 0.0517(16) Uani 1 1 d . . .
H24A H -0.3136 0.1332 0.9020 0.078 Uiso 1 1 calc R . .
H24B H -0.3563 0.1665 0.7390 0.078 Uiso 1 1 calc R . .
H24C H -0.3371 0.1904 0.9309 0.078 Uiso 1 1 calc R . .
N5 N 0.1322(12) 0.5065(7) 0.772(2) 0.099(3) Uiso 0.50 1 d PD . .
C25 C 0.2150(12) 0.5077(8) 0.788(3) 0.099(3) Uiso 0.50 1 d PD . .
C26 C 0.3165(13) 0.4855(8) 0.820(3) 0.099(3) Uiso 0.50 1 d PD . .
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'
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'
I I -0.4742 1.8119 '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
Cu1 I1 Cu1 98.61(3) 4_566 .
N1 Cu1 N3 93.95(18) . .
N1 Cu1 I1 116.30(13) . 4_565
N3 Cu1 I1 111.00(13) . 4_565
N1 Cu1 I1 106.27(12) . .
N3 Cu1 I1 112.12(13) . .
I1 Cu1 I1 115.27(3) 4_565 .
C1 S1 C13 111.0(3) . .
C1 N1 C2 114.3(5) . .
C1 N1 Cu1 123.2(4) . .
C2 N1 Cu1 121.7(4) . .
C1 N2 C4 118.8(5) . .
C14 N3 C13 114.4(5) . .
C14 N3 Cu1 121.2(4) . .
C13 N3 Cu1 124.1(4) . .
C13 N4 C16 117.8(5) . .
N2 C1 N1 125.9(5) . .
N2 C1 S1 109.7(4) . .
N1 C1 S1 124.3(4) . .
N1 C2 C3 125.0(5) . .
C2 C3 C4 115.2(5) . .
C2 C3 C5 121(5) . .
C4 C3 C5 124(5) . .
C2 C3 C5A 118(5) . .
C4 C3 C5A 126(5) . .
C5 C3 C5A 12(5) . .
N2 C4 C3 120.5(5) . .
N2 C4 C6 114.9(5) . .
C3 C4 C6 124.5(5) . .
C7 C6 C11 119.4(6) . .
C7 C6 C4 117.8(5) . .
C11 C6 C4 122.8(6) . .
C8 C7 C6 120.3(6) . .
C7 C8 C9 121.0(6) . .
C10 C9 C8 118.1(5) . .
C10 C9 C12 113.9(18) . .
C8 C9 C12 128.0(18) . .
C10 C9 C12A 129.8(16) . .
C8 C9 C12A 112.1(16) . .
C12 C9 C12A 16.1(8) . .
C11 C10 C9 121.1(6) . .
C10 C11 C6 120.0(6) . .
N4 C13 N3 126.8(5) . .
N4 C13 S1 109.7(4) . .
N3 C13 S1 123.4(4) . .
N3 C14 C15 124.8(5) . .
C14 C15 C16 116.1(5) . .
C14 C15 C17 119.8(5) . .
C16 C15 C17 124.0(5) . .
N4 C16 C15 119.7(5) . .
N4 C16 C18 115.9(5) . .
C15 C16 C18 124.3(5) . .
C23 C18 C19 119.1(5) . .
C23 C18 C16 121.8(5) . .
C19 C18 C16 119.1(5) . .
C20 C19 C18 120.8(5) . .
C19 C20 C21 120.7(5) . .
C22 C21 C20 117.5(5) . .
C22 C21 C24 121.8(5) . .
C20 C21 C24 120.7(5) . .
C21 C22 C23 121.8(5) . .
C18 C23 C22 120.0(5) . .
N5 C25 C26 155(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.5619(9) 4_566
I1 Cu1 2.5856(11) .
Cu1 N1 2.057(4) .
Cu1 N3 2.067(4) .
Cu1 I1 2.5619(9) 4_565
S1 C1 1.770(6) .
S1 C13 1.779(5) .
N1 C1 1.338(7) .
N1 C2 1.345(7) .
N2 C1 1.326(7) .
N2 C4 1.338(7) .
N3 C14 1.332(7) .
N3 C13 1.333(7) .
N4 C13 1.329(7) .
N4 C16 1.346(7) .
C2 C3 1.382(8) .
C3 C4 1.405(8) .
C3 C5 1.512(10) .
C3 C5A 1.512(10) .
C4 C6 1.498(8) .
C6 C7 1.388(9) .
C6 C11 1.390(9) .
C7 C8 1.382(8) .
C8 C9 1.400(8) .
C9 C10 1.392(9) .
C9 C12 1.517(9) .
C9 C12A 1.524(8) .
C10 C11 1.389(8) .
C14 C15 1.373(8) .
C15 C16 1.412(8) .
C15 C17 1.529(8) .
C16 C18 1.484(8) .
C18 C23 1.381(7) .
C18 C19 1.392(8) .
C19 C20 1.387(8) .
C20 C21 1.402(8) .
C21 C22 1.390(8) .
C21 C24 1.497(8) .
C22 C23 1.392(8) .
N5 C25 1.120(9) .
C25 C26 1.495(10) .
