#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:23:24 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178605 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/16/4071699.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_4071699
loop_
_publ_author_name
'Kelly, Mairéad E.'
'Dietrich, Andrea'
'Gómez-Ruiz, Santiago'
'Kalinowski, Bernd'
'Kaluderović, Goran N.'
'Müller, Thomas'
'Paschke, Reinhard'
'Schmidt, Jürgen'
'Steinborn, Dirk'
'Wagner, Christoph'
'Schmidt, Harry'
_publ_section_title
;
 Platinum(IV) Metallacrown Ethers: Synthesis, Structures, Host Properties
 and Anticancer Evaluation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4917
_journal_paper_doi               10.1021/om800323z
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C24 H40 Br4 N8 O2 Pt2, 2(C4 H8 O)'
_chemical_formula_sum            'C32 H56 Br4 N8 O4 Pt2'
_chemical_formula_weight         1326.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.14(3)
_cell_angle_beta                 91.04(3)
_cell_angle_gamma                105.57(3)
_cell_formula_units_Z            1
_cell_length_a                   8.669(2)
_cell_length_b                   11.457(3)
_cell_length_c                   12.083(3)
_cell_measurement_reflns_used    7270
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.0
_cell_volume                     1077.2(6)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1999)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'Diamond (Brandenburg, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'area detector'
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8061
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    10.238
_exptl_absorpt_correction_T_max  0.5220
_exptl_absorpt_correction_T_min  0.2410
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'IPDS (Stoe & Cie, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0421
_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)+(0.0557P)²+5.3336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                3127
_reflns_number_total             3839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800323z_si_002.cif
_cod_data_source_block           z:\ipds28\ipds2865
_cod_original_cell_volume        1077.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4071699
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.4332(13) 0.5810(8) 0.2221(8) 0.042(2) Uani 1 1 d .
H1 H 0.4042 0.5208 0.1416 0.050 Uiso 1 1 calc R
H2 H 0.3462 0.5635 0.2676 0.050 Uiso 1 1 calc R
H3 H 0.5282 0.5716 0.2558 0.050 Uiso 1 1 calc R
C2 C 0.6577(13) 0.8288(9) 0.3628(8) 0.046(2) Uani 1 1 d .
H6 H 0.6912 0.9219 0.3991 0.056 Uiso 1 1 calc R
H5 H 0.7481 0.7995 0.3333 0.056 Uiso 1 1 calc R
H4 H 0.6174 0.7919 0.4206 0.056 Uiso 1 1 calc R
C3 C 0.5234(14) 1.0709(8) 0.3247(7) 0.046(2) Uani 1 1 d .
H7 H 0.5000 1.0668 0.3983 0.055 Uiso 1 1 calc R
C4 C 0.5678(16) 1.0173(9) 0.1415(8) 0.058(3) Uani 1 1 d .
H8 H 0.5810 0.9682 0.0650 0.069 Uiso 1 1 calc R
C5 C 0.5876(17) 1.1459(10) 0.1827(8) 0.059(3) Uani 1 1 d .
H9 H 0.6145 1.2009 0.1401 0.071 Uiso 1 1 calc R
C6 C 0.5677(16) 1.3105(9) 0.3850(10) 0.060(3) Uani 1 1 d .
H10 H 0.5354 1.3033 0.4594 0.072 Uiso 1 1 calc R
H11 H 0.4917 1.3436 0.3540 0.072 Uiso 1 1 calc R
C7 C 0.7313(18) 1.4041(10) 0.4078(8) 0.066(4) Uani 1 1 d .
H13 H 0.7379 1.4818 0.4761 0.079 Uiso 1 1 calc R
H12 H 0.8118 1.3655 0.4239 0.079 Uiso 1 1 calc R
C8 C 0.9171(17) 1.4982(12) 0.3024(9) 0.070(4) Uani 1 1 d .
H14 H 0.9826 1.4409 0.2994 0.084 Uiso 1 1 calc R
H15 H 0.9557 1.5747 0.3742 0.084 Uiso 1 1 calc R
C9 C 0.9333(14) 1.5380(10) 0.1951(8) 0.053(3) Uani 1 1 d .
H17 H 0.8759 1.6016 0.2021 0.064 Uiso 1 1 calc R
H16 H 1.0462 1.5782 0.1925 0.064 Uiso 1 1 calc R
C10 C 0.7340(12) 1.3995(8) 0.0183(8) 0.038(2) Uani 1 1 d .
H18 H 0.6623 1.4490 0.0372 0.046 Uiso 1 1 calc R
C11 C 0.9387(16) 1.3308(12) 0.0282(9) 0.061(3) Uani 1 1 d .
H19 H 1.0362 1.3237 0.0542 0.074 Uiso 1 1 calc R
C12 C 0.8397(14) 1.2496(11) -0.0723(8) 0.054(3) Uani 1 1 d .
H20 H 0.8564 1.1756 -0.1275 0.065 Uiso 1 1 calc R
C13 C 0.043(4) 1.160(2) 0.3869(18) 0.152(10) Uani 1 1 d .
H21 H 0.0961 1.1579 0.4572 0.182 Uiso 1 1 calc R
H22 H -0.0640 1.1684 0.4028 0.182 Uiso 1 1 calc R
C14 C 0.031(4) 1.049(2) 0.292(2) 0.174(13) Uani 1 1 d .
H24 H -0.0802 0.9948 0.2710 0.209 Uiso 1 1 calc R
H23 H 0.0960 1.0002 0.3115 0.209 Uiso 1 1 calc R
C15 C 0.089(4) 1.087(3) 0.192(2) 0.164(11) Uani 1 1 d .
H25 H 0.1844 1.0607 0.1682 0.197 Uiso 1 1 calc R
H26 H 0.0063 1.0496 0.1245 0.197 Uiso 1 1 calc R
C16 C 0.124(4) 1.220(3) 0.239(2) 0.182(14) Uani 1 1 d .
H27 H 0.2258 1.2581 0.2154 0.218 Uiso 1 1 calc R
H28 H 0.0409 1.2454 0.2068 0.218 Uiso 1 1 calc R
N1 N 0.5249(10) 0.9696(6) 0.2301(6) 0.0378(17) Uani 1 1 d .
N2 N 0.5602(12) 1.1810(7) 0.3005(6) 0.049(2) Uani 1 1 d .
N3 N 0.7119(9) 1.2950(7) -0.0783(6) 0.0357(16) Uani 1 1 d .
N4 N 0.8681(10) 1.4251(8) 0.0840(7) 0.0436(19) Uani 1 1 d .
O1 O 0.7585(11) 1.4357(7) 0.3050(6) 0.061(2) Uani 1 1 d .
O2 O 0.134(2) 1.2652(13) 0.3568(16) 0.162(7) Uani 1 1 d .
Br1 Br 0.67707(13) 0.73297(9) 0.08196(8) 0.0469(3) Uani 1 1 d .
Br2 Br 0.28273(13) 0.80704(8) 0.36973(7) 0.0445(2) Uani 1 1 d .
Pt Pt 0.47914(4) 0.77116(3) 0.22486(3) 0.03382(14) 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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
Pt C1 H1 109.5 . .
Pt C1 H2 109.5 . .
H1 C1 H2 109.5 . .
Pt C1 H3 109.5 . .
H1 C1 H3 109.5 . .
H2 C1 H3 109.5 . .
Pt C2 H6 109.5 . .
Pt C2 H5 109.5 . .
H6 C2 H5 109.5 . .
Pt C2 H4 109.5 . .
H6 C2 H4 109.5 . .
H5 C2 H4 109.5 . .
N1 C3 N2 111.2(7) . .
N1 C3 H7 124.4 . .
N2 C3 H7 124.4 . .
C5 C4 N1 109.4(8) . .
C5 C4 H8 125.3 . .
N1 C4 H8 125.3 . .
C4 C5 N2 107.0(8) . .
C4 C5 H9 126.5 . .
N2 C5 H9 126.5 . .
N2 C6 C7 112.6(9) . .
N2 C6 H10 109.1 . .
C7 C6 H10 109.1 . .
N2 C6 H11 109.1 . .
C7 C6 H11 109.1 . .
H10 C6 H11 107.8 . .
O1 C7 C6 107.4(10) . .
O1 C7 H13 110.2 . .
C6 C7 H13 110.2 . .
O1 C7 H12 110.2 . .
C6 C7 H12 110.2 . .
H13 C7 H12 108.5 . .
O1 C8 C9 110.3(10) . .
O1 C8 H14 109.6 . .
C9 C8 H14 109.6 . .
O1 C8 H15 109.6 . .
C9 C8 H15 109.6 . .
H14 C8 H15 108.1 . .
N4 C9 C8 111.4(8) . .
N4 C9 H17 109.4 . .
C8 C9 H17 109.4 . .
N4 C9 H16 109.4 . .
C8 C9 H16 109.4 . .
H17 C9 H16 108.0 . .
N4 C10 N3 111.8(8) . .
N4 C10 H18 124.1 . .
N3 C10 H18 124.1 . .
C12 C11 N4 106.9(11) . .
C12 C11 H19 126.5 . .
N4 C11 H19 126.5 . .
C11 C12 N3 108.0(9) . .
C11 C12 H20 126.0 . .
N3 C12 H20 126.0 . .
C14 C13 O2 106.8(18) . .
C14 C13 H21 110.4 . .
O2 C13 H21 110.4 . .
C14 C13 H22 110.4 . .
O2 C13 H22 110.4 . .
H21 C13 H22 108.6 . .
C13 C14 C15 108(2) . .
C13 C14 H24 110.1 . .
C15 C14 H24 110.1 . .
C13 C14 H23 110.1 . .
C15 C14 H23 110.1 . .
H24 C14 H23 108.4 . .
C16 C15 C14 102.6(18) . .
C16 C15 H25 111.3 . .
C14 C15 H25 111.3 . .
C16 C15 H26 111.3 . .
C14 C15 H26 111.3 . .
H25 C15 H26 109.2 . .
O2 C16 C15 112(2) . .
O2 C16 H27 109.1 . .
C15 C16 H27 109.1 . .
O2 C16 H28 109.1 . .
C15 C16 H28 109.1 . .
H27 C16 H28 107.9 . .
C3 N1 C4 106.1(7) . .
C3 N1 Pt 125.2(6) . .
C4 N1 Pt 128.6(6) . .
C3 N2 C5 106.4(7) . .
C3 N2 C6 125.4(7) . .
C5 N2 C6 128.2(8) . .
C10 N3 C12 106.3(8) . .
C10 N3 Pt 124.9(6) . 2_675
C12 N3 Pt 128.5(6) . 2_675
C10 N4 C11 107.0(9) . .
C10 N4 C9 126.0(9) . .
C11 N4 C9 127.0(10) . .
C8 O1 C7 113.7(9) . .
C16 O2 C13 105.5(18) . .
C2 Pt C1 88.2(4) . .
C2 Pt N1 91.6(3) . .
C1 Pt N1 179.1(3) . .
C2 Pt N3 178.6(3) . 2_675
C1 Pt N3 90.4(3) . 2_675
N1 Pt N3 89.8(3) . 2_675
C2 Pt Br1 89.9(3) . .
C1 Pt Br1 90.3(3) . .
N1 Pt Br1 90.55(19) . .
N3 Pt Br1 90.13(18) 2_675 .
C2 Pt Br2 89.4(3) . .
C1 Pt Br2 88.9(3) . .
N1 Pt Br2 90.27(19) . .
N3 Pt Br2 90.52(18) 2_675 .
Br1 Pt Br2 178.96(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Pt 2.095(8) .
C1 H1 0.9600 .
C1 H2 0.9600 .
C1 H3 0.9600 .
C2 Pt 2.052(10) .
C2 H6 0.9600 .
C2 H5 0.9600 .
C2 H4 0.9600 .
C3 N1 1.323(10) .
C3 N2 1.348(11) .
C3 H7 0.9300 .
C4 C5 1.344(13) .
C4 N1 1.375(11) .
C4 H8 0.9300 .
C5 N2 1.383(11) .
C5 H9 0.9300 .
C6 N2 1.466(11) .
C6 C7 1.485(18) .
C6 H10 0.9700 .
C6 H11 0.9700 .
C7 O1 1.416(11) .
C7 H13 0.9700 .
C7 H12 0.9700 .
C8 O1 1.376(15) .
C8 C9 1.512(14) .
C8 H14 0.9700 .
C8 H15 0.9700 .
C9 N4 1.476(12) .
C9 H17 0.9700 .
C9 H16 0.9700 .
C10 N4 1.301(13) .
C10 N3 1.320(11) .
C10 H18 0.9300 .
C11 C12 1.354(16) .
C11 N4 1.365(13) .
C11 H19 0.9300 .
C12 N3 1.355(13) .
C12 H20 0.9300 .
C13 C14 1.36(3) .
C13 O2 1.42(3) .
C13 H21 0.9700 .
C13 H22 0.9700 .
C14 C15 1.47(3) .
C14 H24 0.9700 .
C14 H23 0.9700 .
C15 C16 1.37(3) .
C15 H25 0.9700 .
C15 H26 0.9700 .
C16 O2 1.33(2) .
C16 H27 0.9700 .
C16 H28 0.9700 .
N1 Pt 2.179(7) .
N3 Pt 2.179(7) 2_675
Br1 Pt 2.4714(12) .
Br2 Pt 2.4741(12) .
Pt N3 2.179(8) 2_675
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_4
N1 C4 C5 N2 1.3(15) .
N2 C6 C7 O1 72.5(12) .
O1 C8 C9 N4 -56.4(14) .
N4 C11 C12 N3 0.9(12) .
O2 C13 C14 C15 -11(3) .
C13 C14 C15 C16 -2(4) .
C14 C15 C16 O2 16(4) .
N2 C3 N1 C4 1.2(13) .
N2 C3 N1 Pt 178.4(7) .
C5 C4 N1 C3 -1.6(14) .
C5 C4 N1 Pt -178.7(8) .
N1 C3 N2 C5 -0.4(13) .
N1 C3 N2 C6 179.3(11) .
C4 C5 N2 C3 -0.6(14) .
C4 C5 N2 C6 179.7(12) .
C7 C6 N2 C3 117.7(12) .
C7 C6 N2 C5 -62.6(17) .
N4 C10 N3 C12 1.2(10) .
N4 C10 N3 Pt -171.9(5) 2_675
C11 C12 N3 C10 -1.3(11) .
C11 C12 N3 Pt 171.6(7) 2_675
N3 C10 N4 C11 -0.7(11) .
N3 C10 N4 C9 177.1(8) .
C12 C11 N4 C10 -0.1(12) .
C12 C11 N4 C9 -177.9(9) .
C8 C9 N4 C10 107.0(12) .
C8 C9 N4 C11 -75.7(14) .
C9 C8 O1 C7 -175.4(9) .
C6 C7 O1 C8 -166.2(10) .
C15 C16 O2 C13 -23(4) .
C14 C13 O2 C16 20(3) .
C3 N1 Pt C2 -55.4(9) .
C4 N1 Pt C2 121.2(10) .
C3 N1 Pt C1 23(24) .
C4 N1 Pt C1 -160(24) .
C3 N1 Pt N3 124.6(9) 2_675
C4 N1 Pt N3 -58.8(10) 2_675
C3 N1 Pt Br1 -145.3(9) .
C4 N1 Pt Br1 31.3(9) .
C3 N1 Pt Br2 34.0(9) .
C4 N1 Pt Br2 -149.4(9) .
