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#$Date: 2016-03-25 13:53:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179869 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/65/7016566.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_7016566
loop_
_publ_author_name
'Lemouchi, C.'
'Barrès, A-L'
'Mézière, C'
'Rondeau, D.'
'Zorina, L.'
'Wzietek, P.'
'Batail, P.'
_publ_section_title
;
 Asymmetric addition of pyridine to
 1,4-bis(ethynyl)bicyclo[2.2.2]octane: dissymmetrical rotator ligands
 illustrated in dpppPt(ii) and [Re(6)Se(8)](2+) complexes and an
 amphidynamic hydrogen bonded framework solid.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8075
_journal_page_last               8078
_journal_paper_doi               10.1039/c1dt10913h
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C17 H18 N), C4 N4 Pt, 2(H2 O)'
_chemical_formula_sum            'C38 H40 N6 O2 Pt'
_chemical_formula_weight         807.85
_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                 109.925(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5093(7)
_cell_length_b                   10.2580(3)
_cell_length_c                   13.9549(6)
_cell_measurement_reflns_used    20763
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     1818.09(15)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       'combined φ and ω-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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49306
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         3.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.899
_exptl_absorpt_correction_T_max  0.361
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0141P)²+1.2071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                4810
_reflns_number_total             7949
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1dt10913h.txt
_cod_data_source_block
(1-pyr-diethynilbicyclo[2,2,2]octaneH+)2[OH2]2[Pt(CN)4]2-
_cod_original_cell_volume        1818.09(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7016566
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
Pt01 Pt 0.0000 0.5000 0.5000 0.03239(3) Uani 1 2 d S
N01 N -0.04775(17) 0.7956(2) 0.44870(16) 0.0509(5) Uani 1 1 d .
N02 N 0.12781(14) 0.4980(2) 0.34931(14) 0.0503(4) Uani 1 1 d .
C02 C 0.08269(14) 0.4974(2) 0.40580(13) 0.0385(4) Uani 1 1 d .
C01 C -0.03108(16) 0.6870(2) 0.46844(16) 0.0411(5) Uani 1 1 d .
C1 C 0.32849(18) 0.8506(2) 0.54390(18) 0.0479(5) Uani 1 1 d .
H1 H 0.2824 0.8767 0.5768 0.057 Uiso 1 1 calc R
C2 C 0.38707(16) 0.8174(2) 0.50200(16) 0.0381(4) Uani 1 1 d .
C3 C 0.46209(15) 0.77145(18) 0.45372(14) 0.0304(4) Uani 1 1 d .
C4 C 0.42408(16) 0.6424(2) 0.39732(16) 0.0389(4) Uani 1 1 d .
H4A H 0.4141 0.5785 0.4444 0.047 Uiso 1 1 calc R
H4B H 0.3569 0.6559 0.3436 0.047 Uiso 1 1 calc R
C5 C 0.47483(16) 0.8712(2) 0.37617(16) 0.0378(4) Uani 1 1 d .
H5A H 0.4067 0.8887 0.3251 0.045 Uiso 1 1 calc R
H5B H 0.5020 0.9524 0.4108 0.045 Uiso 1 1 calc R
C6 C 0.57056(16) 0.7498(2) 0.53508(14) 0.0398(5) Uani 1 1 d .
H6A H 0.5945 0.8302 0.5724 0.048 Uiso 1 1 calc R
H6B H 0.5651 0.6841 0.5831 0.048 Uiso 1 1 calc R
C7 C 0.50451(16) 0.59100(19) 0.35114(15) 0.0358(4) Uani 1 1 d .
H7A H 0.4706 0.5785 0.2783 0.043 Uiso 1 1 calc R
H7B H 0.5314 0.5074 0.3813 0.043 Uiso 1 1 calc R
C8 C 0.55017(16) 0.81952(19) 0.32430(15) 0.0354(4) Uani 1 1 d .
H8A H 0.6068 0.8815 0.3331 0.042 Uiso 1 1 calc R
H8B H 0.5127 0.8092 0.2518 0.042 Uiso 1 1 calc R
C9 C 0.65065(15) 0.7056(2) 0.48615(14) 0.0376(4) Uani 1 1 d .
H9A H 0.6824 0.6239 0.5164 0.045 Uiso 1 1 calc R
H9B H 0.7061 0.7702 0.4987 0.045 Uiso 1 1 calc R
C10 C 0.59593(13) 0.68788(17) 0.37071(12) 0.0266(3) Uani 1 1 d .
C11 C 0.67136(14) 0.63723(19) 0.32576(13) 0.0324(4) Uani 1 1 d .
C12 C 0.73283(15) 0.5909(2) 0.29098(14) 0.0352(4) Uani 1 1 d .
C13 C 0.80154(14) 0.5340(2) 0.24451(14) 0.0368(5) Uani 1 1 d .
C14 C 0.82100(16) 0.4000(2) 0.25088(17) 0.0431(5) Uani 1 1 d .
H14 H 0.7927 0.3472 0.2892 0.052 Uiso 1 1 calc R
C15 C 0.88192(18) 0.3471(3) 0.2003(2) 0.0538(6) Uani 1 1 d .
H15 H 0.8942 0.2577 0.2027 0.065 Uiso 1 1 calc R
N16 N 0.92369(16) 0.4249(3) 0.14738(15) 0.0571(6) Uani 1 1 d .
H16 H 0.9608 0.3898 0.1150 0.069 Uiso 1 1 calc R
C17 C 0.9110(2) 0.5530(3) 0.14204(18) 0.0563(6) Uani 1 1 d .
H17 H 0.9439 0.6035 0.1063 0.068 Uiso 1 1 calc R
C18 C 0.84889(17) 0.6103(3) 0.18959(16) 0.0452(5) Uani 1 1 d .
H18 H 0.8383 0.7000 0.1853 0.054 Uiso 1 1 calc R
O21 O 0.1851(2) 0.9757(3) 0.66711(18) 0.0834(8) Uani 1 1 d D
H21A H 0.176(4) 0.981(4) 0.720(3) 0.125 Uiso 1 1 d D
H21B H 0.164(4) 1.041(3) 0.636(3) 0.125 Uiso 1 1 d 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'
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
C01 Pt01 C01 180.0 . 3_566
C01 Pt01 C02 89.44(9) . .
C01 Pt01 C02 90.56(9) 3_566 .
C01 Pt01 C02 90.56(9) . 3_566
C01 Pt01 C02 89.44(9) 3_566 3_566
C02 Pt01 C02 180.0 . 3_566
N02 C02 Pt01 177.86(18) . .
N01 C01 Pt01 178.44(19) . .
C2 C1 H1 180.0 . .
C1 C2 C3 177.2(2) . .
C2 C3 C6 109.92(16) . .
C2 C3 C4 110.39(16) . .
C6 C3 C4 108.83(16) . .
C2 C3 C5 111.55(16) . .
C6 C3 C5 108.00(17) . .
C4 C3 C5 108.07(16) . .
C7 C4 C3 110.53(16) . .
C7 C4 H4A 109.5 . .
C3 C4 H4A 109.5 . .
C7 C4 H4B 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
C8 C5 C3 110.68(15) . .
C8 C5 H5A 109.5 . .
C3 C5 H5A 109.5 . .
C8 C5 H5B 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
C9 C6 C3 110.78(15) . .
C9 C6 H6A 109.5 . .
C3 C6 H6A 109.5 . .
C9 C6 H6B 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
C4 C7 C10 110.17(15) . .
C4 C7 H7A 109.6 . .
C10 C7 H7A 109.6 . .
C4 C7 H7B 109.6 . .
C10 C7 H7B 109.6 . .
H7A C7 H7B 108.1 . .
C5 C8 C10 110.05(15) . .
C5 C8 H8A 109.7 . .
C10 C8 H8A 109.7 . .
C5 C8 H8B 109.7 . .
C10 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
C6 C9 C10 109.98(15) . .
C6 C9 H9A 109.7 . .
C10 C9 H9A 109.7 . .
C6 C9 H9B 109.7 . .
C10 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
C11 C10 C8 111.80(15) . .
C11 C10 C7 109.25(15) . .
C8 C10 C7 108.10(15) . .
C11 C10 C9 109.58(14) . .
C8 C10 C9 108.60(15) . .
C7 C10 C9 109.48(15) . .
C12 C11 C10 177.2(2) . .
C11 C12 C13 176.9(2) . .
C18 C13 C14 118.41(19) . .
C18 C13 C12 120.8(2) . .
C14 C13 C12 120.75(19) . .
C15 C14 C13 119.4(2) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
N16 C15 C14 119.4(2) . .
N16 C15 H15 120.3 . .
C14 C15 H15 120.3 . .
C17 N16 C15 123.6(2) . .
C17 N16 H16 118.2 . .
C15 N16 H16 118.2 . .
N16 C17 C18 119.2(3) . .
N16 C17 H17 120.4 . .
C18 C17 H17 120.4 . .
C17 C18 C13 119.9(2) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
H21A O21 H21B 108(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt01 C01 1.981(3) .
Pt01 C01 1.981(3) 3_566
Pt01 C02 1.9943(18) .
Pt01 C02 1.9943(18) 3_566
N01 C01 1.151(3) .
N02 C02 1.149(2) .
C1 C2 1.183(3) .
C1 H1 0.9300 .
C2 C3 1.473(3) .
C3 C6 1.533(3) .
C3 C4 1.536(3) .
C3 C5 1.541(3) .
C4 C7 1.534(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C8 1.531(3) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C9 1.531(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C10 1.535(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C10 1.534(2) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.537(2) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.462(2) .
C11 C12 1.194(3) .
C12 C13 1.426(3) .
C13 C18 1.394(3) .
C13 C14 1.397(3) .
C14 C15 1.366(3) .
C14 H14 0.9300 .
C15 N16 1.336(4) .
C15 H15 0.9300 .
N16 C17 1.325(4) .
N16 H16 0.8600 .
C17 C18 1.367(3) .
C17 H17 0.9300 .
C18 H18 0.9300 .
O21 H21A 0.79(3) .
O21 H21B 0.79(3) .
