#------------------------------------------------------------------------------
#$Date: 2018-08-16 01:01:38 +0300 (Thu, 16 Aug 2018) $
#$Revision: 209738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/27/7102776.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_7102776
loop_
_publ_author_name
'Clayton, Hayley J.'
'Harding, Lindsay P.'
'Irvine, John P.'
'Jeffery, John C.'
'Riis-Johannessen, T.'
'Laws, Andrew P.'
'Rice, Craig R.'
'Whitehead, Martina'
_publ_section_title
;
 Metal-specific allosteric activation and deactivation of a diamine
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              108
_journal_page_last               110
_journal_paper_doi               10.1039/b714256k
_journal_year                    2008
_chemical_formula_sum            'C44 H44 Cd2 Cl4 N16 O16 S4'
_chemical_formula_weight         1547.79
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.217(4)
_cell_length_b                   11.429(2)
_cell_length_c                   23.837(5)
_cell_measurement_reflns_used    21560
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.990
_cell_measurement_theta_min      4.773
_cell_volume                     5605.4(19)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'frames each covering 0.3° inω'
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31695
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.883604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0272P)²+9.0361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                6209
_reflns_number_total             6443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714256k.txt
_cod_data_source_block           craigum
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7102776
loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.520563(5) 0.669246(10) 0.855233(5) 0.01455(4) Uani 1 1 d . . .
Cl1 Cl 0.61243(2) 0.44643(4) 0.956459(19) 0.02462(9) Uani 1 1 d . . .
O1A O 0.56891(7) 0.54631(12) 0.94228(6) 0.0294(3) Uani 1 1 d . . .
O1B O 0.67736(7) 0.48646(16) 0.96990(9) 0.0512(5) Uani 1 1 d . . .
O1C O 0.59361(8) 0.36963(14) 0.90507(7) 0.0408(4) Uani 1 1 d . . .
O1D O 0.60803(8) 0.38699(13) 1.00734(6) 0.0374(3) Uani 1 1 d . . .
N51 N 0.50002(7) 0.77927(13) 0.93063(7) 0.0235(3) Uani 1 1 d . . .
C52 C 0.47896(8) 0.81909(15) 0.96301(8) 0.0201(3) Uani 1 1 d . . .
C53 C 0.45181(9) 0.87180(18) 1.00400(8) 0.0240(3) Uani 1 1 d . . .
N11 N 0.62722(6) 0.72905(12) 0.88237(6) 0.0167(3) Uani 1 1 d . . .
C12 C 0.66028(7) 0.65801(15) 0.86136(7) 0.0175(3) Uani 1 1 d . . .
S13 S 0.741975(19) 0.68809(4) 0.88725(2) 0.02258(9) Uani 1 1 d . . .
C14 C 0.73045(8) 0.80269(17) 0.92845(8) 0.0230(3) Uani 1 1 d . . .
C15 C 0.66703(8) 0.81184(15) 0.92132(7) 0.0195(3) Uani 1 1 d . . .
C16 C 0.64032(9) 0.89765(17) 0.95309(8) 0.0250(4) Uani 1 1 d . . .
N21 N 0.56600(6) 0.55147(12) 0.79965(6) 0.0154(3) Uani 1 1 d . . .
C22 C 0.63128(7) 0.56015(14) 0.82063(7) 0.0166(3) Uani 1 1 d . . .
C23 C 0.66885(8) 0.47793(16) 0.80498(7) 0.0199(3) Uani 1 1 d . . .
C24 C 0.63917(8) 0.38567(15) 0.76850(8) 0.0207(3) Uani 1 1 d . . .
C25 C 0.57100(8) 0.37541(15) 0.74557(7) 0.0193(3) Uani 1 1 d . . .
C26 C 0.53617(7) 0.46314(14) 0.76212(7) 0.0158(3) Uani 1 1 d . . .
N27 N 0.54026(9) 0.28507(14) 0.70905(8) 0.0253(3) Uani 1 1 d . . .
N31 N 0.41577(6) 0.60598(12) 0.83980(6) 0.0171(3) Uani 1 1 d . . .
C32 C 0.37237(7) 0.68189(14) 0.80657(7) 0.0169(3) Uani 1 1 d . . .
S33 S 0.29512(2) 0.65526(4) 0.80352(2) 0.02363(9) Uani 1 1 d . . .
C34 C 0.32366(9) 0.53665(17) 0.84973(8) 0.0248(4) Uani 1 1 d . . .
C35 C 0.38856(8) 0.52278(15) 0.86529(7) 0.0206(3) Uani 1 1 d . . .
C36 C 0.42911(10) 0.43096(17) 0.90681(9) 0.0265(4) Uani 1 1 d . . .
N41 N 0.44921(6) 0.78804(12) 0.77850(6) 0.0144(2) Uani 1 1 d . . .
C42 C 0.38736(7) 0.77955(14) 0.77439(7) 0.0157(3) Uani 1 1 d . . .
C43 C 0.34030(8) 0.86007(16) 0.74034(7) 0.0188(3) Uani 1 1 d . . .
C44 C 0.35709(8) 0.94855(15) 0.71072(7) 0.0187(3) Uani 1 1 d . . .
C45 C 0.42129(7) 0.95756(14) 0.71308(7) 0.0167(3) Uani 1 1 d . . .
C46 C 0.46581(7) 0.87284(14) 0.74800(7) 0.0144(3) Uani 1 1 d . . .
N47 N 0.43930(8) 1.04362(14) 0.68361(7) 0.0212(3) Uani 1 1 d . . .
Cl2 Cl 0.380961(18) 0.07322(3) 0.860760(17) 0.01762(8) Uani 1 1 d . . .
O2A O 0.44137(6) 0.03513(12) 0.85685(6) 0.0266(3) Uani 1 1 d . . .
O2B O 0.39459(6) 0.13039(12) 0.91814(6) 0.0267(3) Uani 1 1 d . . .
O2C O 0.34937(7) 0.15368(12) 0.81215(6) 0.0304(3) Uani 1 1 d . . .
O2D O 0.33946(6) -0.02603(12) 0.85583(6) 0.0276(3) Uani 1 1 d . . .
N61 N 0.31107(9) 0.16013(17) 0.60688(9) 0.0384(4) Uani 1 1 d . . .
C62 C 0.27194(9) 0.22806(16) 0.58695(8) 0.0241(3) Uani 1 1 d . . .
C63 C 0.22174(10) 0.31546(18) 0.56110(9) 0.0288(4) Uani 1 1 d . . .
H1 H 0.4749(13) 1.042(2) 0.6826(11) 0.036(7) Uiso 1 1 d . . .
H2 H 0.4331(12) 0.811(2) 1.0194(11) 0.037(6) Uiso 1 1 d . . .
H3 H 0.7655(11) 0.850(2) 0.9513(10) 0.027(6) Uiso 1 1 d . . .
H4 H 0.2980(10) 0.8531(18) 0.7403(9) 0.020(5) Uiso 1 1 d . . .
H5 H 0.7128(11) 0.4859(19) 0.8197(10) 0.026(5) Uiso 1 1 d . . .
H6 H 0.6013(12) 0.928(2) 0.9271(10) 0.029(6) Uiso 1 1 d . . .
H7 H 0.4111(12) 1.083(2) 0.6612(11) 0.030(6) Uiso 1 1 d . . .
H8 H 0.4207(12) 0.930(2) 0.9838(11) 0.039(6) Uiso 1 1 d . . .
H9 H 0.3291(11) 1.003(2) 0.6892(11) 0.033(6) Uiso 1 1 d . . .
H10 H 0.6323(11) 0.863(2) 0.9840(11) 0.033(6) Uiso 1 1 d . . .
H11 H 0.2977(12) 0.491(2) 0.8633(11) 0.042(7) Uiso 1 1 d . . .
H12 H 0.6621(11) 0.3309(19) 0.7580(10) 0.027(6) Uiso 1 1 d . . .
H13 H 0.4589(12) 0.396(2) 0.8905(11) 0.037(6) Uiso 1 1 d . . .
H14 H 0.4854(12) 0.909(2) 1.0364(11) 0.035(6) Uiso 1 1 d . . .
H15 H 0.4551(12) 0.466(2) 0.9443(11) 0.038(6) Uiso 1 1 d . . .
H16 H 0.6722(12) 0.959(2) 0.9706(11) 0.039(7) Uiso 1 1 d . . .
H17 H 0.2434(15) 0.388(3) 0.5571(14) 0.070(10) Uiso 1 1 d . . .
H18 H 0.4028(13) 0.373(2) 0.9134(11) 0.043(7) Uiso 1 1 d . . .
H19 H 0.1993(16) 0.335(3) 0.5870(15) 0.069(10) Uiso 1 1 d . . .
H20 H 0.5632(13) 0.237(2) 0.7017(11) 0.039(7) Uiso 1 1 d . . .
H21 H 0.5037(15) 0.291(3) 0.6900(14) 0.056(9) Uiso 1 1 d . . .
H22 H 0.1939(14) 0.293(3) 0.5231(14) 0.057(8) Uiso 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'
S S 0.1246 0.1234 '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'
Cd Cd -0.8075 1.2024 '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
N11 Cd1 N31 173.37(5) . . ?
N11 Cd1 N41 111.50(5) . . ?
N31 Cd1 N41 73.49(5) . . ?
N11 Cd1 N21 73.50(5) . . ?
N31 Cd1 N21 110.31(5) . . ?
N41 Cd1 N21 101.43(5) . . ?
N11 Cd1 N51 95.80(5) . . ?
N31 Cd1 N51 79.51(5) . . ?
N41 Cd1 N51 90.99(5) . . ?
N21 Cd1 N51 165.88(5) . . ?
N11 Cd1 O1A 81.60(5) . . ?
N31 Cd1 O1A 92.83(5) . . ?
N41 Cd1 O1A 164.37(5) . . ?
N21 Cd1 O1A 90.27(5) . . ?
N51 Cd1 O1A 78.85(5) . . ?
O1D Cl1 O1B 110.44(11) . . ?
O1D Cl1 O1C 110.08(10) . . ?
O1B Cl1 O1C 109.36(12) . . ?
O1D Cl1 O1A 108.63(9) . . ?
O1B Cl1 O1A 109.14(10) . . ?
O1C Cl1 O1A 109.18(9) . . ?
Cl1 O1A Cd1 134.74(8) . . ?
C52 N51 Cd1 166.18(14) . . ?
N51 C52 C53 179.1(2) . . ?
C52 C53 H2 107.9(15) . . ?
C52 C53 H8 110.9(15) . . ?
H2 C53 H8 111(2) . . ?
C52 C53 H14 109.5(14) . . ?
H2 C53 H14 110(2) . . ?
H8 C53 H14 107(2) . . ?
C12 N11 C15 111.72(14) . . ?
C12 N11 Cd1 111.83(11) . . ?
C15 N11 Cd1 135.82(11) . . ?
N11 C12 C22 123.80(14) . . ?
N11 C12 S13 113.97(12) . . ?
C22 C12 S13 122.22(12) . . ?
C14 S13 C12 89.59(9) . . ?
C15 C14 S13 111.07(14) . . ?
C15 C14 H3 128.6(14) . . ?
S13 C14 H3 120.3(14) . . ?
C14 C15 N11 113.65(16) . . ?
C14 C15 C16 125.42(16) . . ?
N11 C15 C16 120.89(15) . . ?
C15 C16 H6 111.1(14) . . ?
C15 C16 H10 111.0(16) . . ?
H6 C16 H10 107(2) . . ?
C15 C16 H16 109.2(15) . . ?
H6 C16 H16 111(2) . . ?
H10 C16 H16 107(2) . . ?
C26 N21 C22 119.54(14) . . ?
C26 N21 Cd1 126.29(10) . . ?
C22 N21 Cd1 112.16(10) . . ?
N21 C22 C23 121.26(15) . . ?
N21 C22 C12 116.47(14) . . ?
C23 C22 C12 122.26(15) . . ?
C24 C23 C22 119.66(15) . . ?
C24 C23 H5 120.8(14) . . ?
C22 C23 H5 119.5(14) . . ?
C23 C24 C25 120.08(16) . . ?
C23 C24 H12 121.7(14) . . ?
C25 C24 H12 118.2(14) . . ?
N27 C25 C24 121.31(16) . . ?
N27 C25 C26 121.59(15) . . ?
C24 C25 C26 117.10(15) . . ?
N21 C26 C25 122.31(14) . . ?
N21 C26 C26 116.53(12) . 2_656 ?
C25 C26 C26 121.15(13) . 2_656 ?
C25 N27 H20 116.5(18) . . ?
C25 N27 H21 118(2) . . ?
H20 N27 H21 123(3) . . ?
C32 N31 C35 112.01(14) . . ?
C32 N31 Cd1 110.59(11) . . ?
C35 N31 Cd1 136.03(11) . . ?
N31 C32 C42 123.96(14) . . ?
N31 C32 S33 113.70(12) . . ?
C42 C32 S33 122.33(12) . . ?
C34 S33 C32 89.52(9) . . ?
C35 C34 S33 111.49(14) . . ?
C35 C34 H11 125.5(16) . . ?
S33 C34 H11 123.0(16) . . ?
C34 C35 N31 113.28(16) . . ?
C34 C35 C36 125.33(16) . . ?
N31 C35 C36 121.37(15) . . ?
C35 C36 H13 110.8(14) . . ?
C35 C36 H15 109.4(15) . . ?
H13 C36 H15 106(2) . . ?
C35 C36 H18 110.7(16) . . ?
H13 C36 H18 110(2) . . ?
H15 C36 H18 110(2) . . ?
C42 N41 C46 119.63(13) . . ?
C42 N41 Cd1 112.73(10) . . ?
C46 N41 Cd1 126.58(10) . . ?
N41 C42 C43 120.96(15) . . ?
N41 C42 C32 116.48(14) . . ?
C43 C42 C32 122.55(14) . . ?
C44 C43 C42 119.84(15) . . ?
C44 C43 H4 122.0(13) . . ?
C42 C43 H4 118.1(13) . . ?
C43 C44 C45 120.26(15) . . ?
C43 C44 H9 123.0(16) . . ?
C45 C44 H9 116.7(16) . . ?
N47 C45 C46 121.77(15) . . ?
N47 C45 C44 121.67(15) . . ?
C46 C45 C44 116.56(15) . . ?
N41 C46 C45 122.69(14) . . ?
N41 C46 C46 116.61(12) . 2_656 ?
C45 C46 C46 120.70(13) . 2_656 ?
C45 N47 H1 119.3(18) . . ?
C45 N47 H7 116.7(17) . . ?
H1 N47 H7 122(2) . . ?
O2C Cl2 O2D 109.61(9) . . ?
O2C Cl2 O2B 109.80(9) . . ?
O2D Cl2 O2B 109.50(8) . . ?
O2C Cl2 O2A 108.85(8) . . ?
O2D Cl2 O2A 109.81(8) . . ?
O2B Cl2 O2A 109.25(8) . . ?
N61 C62 C63 179.7(2) . . ?
C62 C63 H17 107.2(19) . . ?
C62 C63 H19 113.2(19) . . ?
H17 C63 H19 105(3) . . ?
C62 C63 H22 110.3(19) . . ?
H17 C63 H22 108(3) . . ?
H19 C63 H22 112(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
Cd1 N11 2.3116(14) . ?
Cd1 N31 2.3307(14) . ?
Cd1 N41 2.3481(15) . ?
Cd1 N21 2.3656(14) . ?
Cd1 N51 2.3747(15) . ?
Cd1 O1A 2.3982(14) . ?
Cl1 O1D 1.4255(14) . ?
Cl1 O1B 1.4297(16) . ?
Cl1 O1C 1.4351(16) . ?
Cl1 O1A 1.4511(14) . ?
N51 C52 1.138(2) . ?
C52 C53 1.458(2) . ?
C53 H2 0.95(3) . ?
C53 H8 0.95(3) . ?
C53 H14 0.95(2) . ?
N11 C12 1.314(2) . ?
N11 C15 1.386(2) . ?
C12 C22 1.462(2) . ?
C12 S13 1.7171(17) . ?
S13 C14 1.713(2) . ?
C14 C15 1.358(2) . ?
C14 H3 0.94(2) . ?
C15 C16 1.492(3) . ?
C16 H6 0.92(2) . ?
C16 H10 0.91(3) . ?
C16 H16 0.97(3) . ?
N21 C26 1.346(2) . ?
N21 C22 1.347(2) . ?
C22 C23 1.398(2) . ?
C23 C24 1.368(3) . ?
C23 H5 0.91(2) . ?
C24 C25 1.408(2) . ?
C24 H12 0.90(2) . ?
C25 N27 1.357(2) . ?
C25 C26 1.411(2) . ?
C26 C26 1.489(3) 2_656 ?
N27 H20 0.81(3) . ?
N27 H21 0.77(3) . ?
N31 C32 1.317(2) . ?
N31 C35 1.384(2) . ?
C32 C42 1.462(2) . ?
C32 S33 1.7172(16) . ?
S33 C34 1.711(2) . ?
C34 C35 1.356(2) . ?
C34 H11 0.92(3) . ?
C35 C36 1.490(3) . ?
C36 H13 0.97(3) . ?
C36 H15 0.95(3) . ?
C36 H18 0.94(3) . ?
N41 C42 1.3437(19) . ?
N41 C46 1.344(2) . ?
C42 C43 1.399(2) . ?
C43 C44 1.364(2) . ?
C43 H4 0.94(2) . ?
C44 C45 1.410(2) . ?
C44 H9 0.89(2) . ?
C45 N47 1.354(2) . ?
C45 C46 1.410(2) . ?
C46 C46 1.486(3) 2_656 ?
N47 H1 0.80(3) . ?
N47 H7 0.79(2) . ?
Cl2 O2C 1.4377(14) . ?
Cl2 O2D 1.4384(13) . ?
Cl2 O2B 1.4411(13) . ?
Cl2 O2A 1.4471(13) . ?
N61 C62 1.128(3) . ?
C62 C63 1.450(3) . ?
C63 H17 0.98(4) . ?
C63 H19 0.95(3) . ?
C63 H22 0.92(3) . ?
