#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:44:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179075 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/37/4303775.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_4303775
loop_
_publ_author_name
'So Young Lee'
'Sunhong Park'
'Shim Sung Lee'
_publ_contact_author_address
;
Department of Chemistry and Research Institute of Natural Science, 
Gyeongsang National University, Jinju 660-701, South Korea
;
_publ_contact_author_email       sslee@gnu.ac.kr
_publ_contact_author_fax         +82-55-753-7614
_publ_contact_author_name        'Shim Sung Lee'
_publ_contact_author_phone       +82-55-751-6021
_publ_section_title
;
Copper(I), Silver(I), and Palladium(II) Complexes of a Thiaoxamacrocycle
Displaying Unusual Topologies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11335
_journal_page_last               11341
_journal_paper_doi               10.1021/ic901902t
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C18 H20 Br Cu O2 S2'
_chemical_formula_weight         475.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5981(8)
_cell_length_b                   8.3384(6)
_cell_length_c                   19.4876(14)
_cell_measurement_reflns_used    3641
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.66
_cell_volume                     1867.5(2)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11300
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_T_max  0.6187
_exptl_absorpt_correction_T_min  0.3705
_exptl_absorpt_correction_type   'empirical SADABS'
_exptl_absorpt_process_details
;
 Ratio of minimum to maximum apparent transmission:  0.728129
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0321
_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)+(0.0237P)²+0.4071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                3104
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901902t_si_001_2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303775
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.97661(3) -0.15352(5) 0.031348(18) 0.02403(11) Uani 1 1 d . . .
Br1 Br 0.91626(3) 0.11716(4) 0.066672(16) 0.02391(9) Uani 1 1 d . . .
S1 S 1.08962(7) -0.28978(10) 0.11928(4) 0.02461(18) Uani 1 1 d . . .
S2 S 0.81870(7) -0.32750(9) 0.03102(4) 0.02358(18) Uani 1 1 d . . .
O1 O 0.71586(18) -0.2674(3) 0.20846(11) 0.0259(5) Uani 1 1 d . . .
O2 O 0.92312(18) -0.3989(3) 0.27762(11) 0.0294(5) Uani 1 1 d . . .
C1 C 0.7255(3) -0.3235(4) 0.27850(16) 0.0320(8) Uani 1 1 d . . .
H1A H 0.7052 -0.4388 0.2792 0.038 Uiso 1 1 calc R . .
H1B H 0.6714 -0.2634 0.3042 0.038 Uiso 1 1 calc R . .
C2 C 0.8481(3) -0.2987(4) 0.31160(17) 0.0328(8) Uani 1 1 d . . .
H2A H 0.8704 -0.1848 0.3074 0.039 Uiso 1 1 calc R . .
H2B H 0.8554 -0.3263 0.3614 0.039 Uiso 1 1 calc R . .
C3 C 1.0410(3) -0.3762(4) 0.30017(16) 0.0266(7) Uani 1 1 d . . .
C4 C 1.0924(3) -0.4571(4) 0.35950(16) 0.0331(8) Uani 1 1 d . . .
H4A H 1.0470 -0.5242 0.3848 0.040 Uiso 1 1 calc R . .
C5 C 1.2105(3) -0.4376(4) 0.38073(17) 0.0360(9) Uani 1 1 d . . .
H5A H 1.2468 -0.4932 0.4204 0.043 Uiso 1 1 calc R . .
C6 C 1.2758(3) -0.3378(4) 0.34450(18) 0.0363(9) Uani 1 1 d . . .
H6A H 1.3561 -0.3222 0.3603 0.044 Uiso 1 1 calc R . .
C7 C 1.2247(3) -0.2607(4) 0.28556(17) 0.0292(8) Uani 1 1 d . . .
H7A H 1.2708 -0.1947 0.2603 0.035 Uiso 1 1 calc R . .
C8 C 1.1054(3) -0.2787(4) 0.26245(16) 0.0235(7) Uani 1 1 d . . .
C9 C 1.0522(3) -0.1954(4) 0.19760(15) 0.0250(7) Uani 1 1 d . . .
H9A H 1.0787 -0.0825 0.1990 0.030 Uiso 1 1 calc R . .
H9B H 0.9665 -0.1951 0.1959 0.030 Uiso 1 1 calc R . .
C10 C 1.0057(3) -0.4734(4) 0.11586(17) 0.0270(7) Uani 1 1 d . . .
H10A H 1.0268 -0.5401 0.0774 0.032 Uiso 1 1 calc R . .
H10B H 1.0284 -0.5334 0.1594 0.032 Uiso 1 1 calc R . .
C11 C 0.8736(3) -0.4515(4) 0.10583(16) 0.0264(7) Uani 1 1 d . . .
H11A H 0.8506 -0.4019 0.1481 0.032 Uiso 1 1 calc R . .
H11B H 0.8364 -0.5584 0.1003 0.032 Uiso 1 1 calc R . .
C12 C 0.7180(3) -0.1952(4) 0.06883(16) 0.0226(7) Uani 1 1 d . . .
H12A H 0.7624 -0.1366 0.1080 0.027 Uiso 1 1 calc R . .
H12B H 0.6880 -0.1146 0.0336 0.027 Uiso 1 1 calc R . .
C13 C 0.6159(3) -0.2752(4) 0.09456(16) 0.0235(7) Uani 1 1 d . . .
C14 C 0.5169(3) -0.3118(4) 0.04938(19) 0.0346(8) Uani 1 1 d . . .
H14A H 0.5164 -0.2930 0.0013 0.042 Uiso 1 1 calc R . .
C15 C 0.4181(3) -0.3752(4) 0.0723(2) 0.0424(9) Uani 1 1 d . . .
H15A H 0.3515 -0.4014 0.0404 0.051 Uiso 1 1 calc R . .
C16 C 0.4187(3) -0.3994(4) 0.1422(2) 0.0416(10) Uani 1 1 d . . .
H16A H 0.3511 -0.4413 0.1584 0.050 Uiso 1 1 calc R . .
C17 C 0.5155(3) -0.3641(4) 0.1896(2) 0.0339(8) Uani 1 1 d . . .
H17A H 0.5142 -0.3802 0.2377 0.041 Uiso 1 1 calc R . .
C18 C 0.6152(3) -0.3045(4) 0.16534(17) 0.0254(7) 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'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
S1 Cu1 S2 93.60(3) . . ?
S1 Cu1 Br1 110.16(3) . 3_755 ?
S2 Cu1 Br1 123.93(3) . 3_755 ?
S1 Cu1 Br1 113.17(3) . . ?
S2 Cu1 Br1 108.33(3) . . ?
Br1 Cu1 Br1 107.251(16) 3_755 . ?
S1 Cu1 Cu1 128.52(3) . 3_755 ?
S2 Cu1 Cu1 137.18(3) . 3_755 ?
Br1 Cu1 Cu1 54.472(14) 3_755 3_755 ?
Br1 Cu1 Cu1 52.779(15) . 3_755 ?
Cu1 Br1 Cu1 72.749(16) 3_755 . ?
C10 S1 C9 102.04(15) . . ?
C10 S1 Cu1 98.06(10) . . ?
C9 S1 Cu1 103.50(10) . . ?
C11 S2 C12 101.10(14) . . ?
C11 S2 Cu1 99.21(10) . . ?
C12 S2 Cu1 99.60(10) . . ?
C18 O1 C1 117.3(2) . . ?
C3 O2 C2 114.0(2) . . ?
O1 C1 C2 108.3(3) . . ?
O2 C2 C1 108.7(3) . . ?
C8 C3 O2 119.4(3) . . ?
C8 C3 C4 121.5(3) . . ?
O2 C3 C4 119.1(3) . . ?
C5 C4 C3 118.9(3) . . ?
C6 C5 C4 120.4(3) . . ?
C7 C6 C5 120.2(3) . . ?
C6 C7 C8 120.8(3) . . ?
C3 C8 C7 118.2(3) . . ?
C3 C8 C9 122.0(3) . . ?
C7 C8 C9 119.8(3) . . ?
C8 C9 S1 112.9(2) . . ?
C11 C10 S1 115.3(2) . . ?
C10 C11 S2 113.9(2) . . ?
C13 C12 S2 116.1(2) . . ?
C14 C13 C18 118.3(3) . . ?
C14 C13 C12 120.6(3) . . ?
C18 C13 C12 121.0(3) . . ?
C13 C14 C15 121.9(3) . . ?
C16 C15 C14 118.7(3) . . ?
C15 C16 C17 121.5(3) . . ?
C16 C17 C18 118.9(3) . . ?
O1 C18 C17 123.0(3) . . ?
O1 C18 C13 116.4(3) . . ?
C17 C18 C13 120.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S1 2.3109(9) . ?
Cu1 S2 2.3358(9) . ?
Cu1 Br1 2.4339(5) 3_755 ?
Cu1 Br1 2.4875(5) . ?
Cu1 Cu1 2.9190(8) 3_755 ?
Br1 Cu1 2.4339(5) 3_755 ?
S1 C10 1.811(3) . ?
S1 C9 1.821(3) . ?
S2 C11 1.831(3) . ?
S2 C12 1.832(3) . ?
O1 C18 1.379(4) . ?
O1 C1 1.433(4) . ?
O2 C3 1.391(4) . ?
O2 C2 1.432(4) . ?
C1 C2 1.495(4) . ?
C3 C8 1.381(4) . ?
C3 C4 1.400(4) . ?
C4 C5 1.386(5) . ?
C5 C6 1.381(5) . ?
C6 C7 1.378(4) . ?
C7 C8 1.405(4) . ?
C8 C9 1.500(4) . ?
C10 C11 1.529(4) . ?
C12 C13 1.504(4) . ?
C13 C14 1.383(4) . ?
C13 C18 1.402(4) . ?
C14 C15 1.389(5) . ?
C15 C16 1.376(5) . ?
C16 C17 1.386(5) . ?
C17 C18 1.397(4) . ?
