#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:47:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180155 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/51/7105157.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_7105157
loop_
_publ_author_name
'Flores-Figueroa, Aarón'
'Pape, Tania'
'Feldmann, Kai-Oliver'
'Hahn, F Ekkehardt'
_publ_section_title
;
 Template-controlled synthesis of a planar [16]ane-P2C(NHC)2
 macrocycle.
;
_journal_issue                   2
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              324
_journal_page_last               326
_journal_paper_doi               10.1039/b920474a
_journal_volume                  46
_journal_year                    2009
_chemical_formula_sum            'C12 H34 Cl2 N4 O2 P2 Pt'
_chemical_formula_weight         594.36
_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                109.1550(10)
_cell_angle_beta                 106.7150(10)
_cell_angle_gamma                107.2700(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3796(7)
_cell_length_b                   8.5616(7)
_cell_length_c                   9.4705(12)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     554.25(10)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5893
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    6.726
_exptl_absorpt_correction_T_max  0.6503
_exptl_absorpt_correction_T_min  0.2737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Corrections were done with the SADABS program, utilizing the none merged
raw data obtained from the integration process. Integration and final cell
refinement were done with SAINT.

SADABS reports ratio of Tmin/Tmax = 0.539496

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plates'
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.968
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0186
_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)+(0.0349P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                2805
_reflns_number_total             2805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920474a.txt
_cod_data_source_block           6a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105157
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.5000 1.0000 0.5000 0.01447(5) Uani 1 2 d S . .
P2 P 0.60424(9) 0.91777(8) 0.70522(8) 0.01737(12) Uani 1 1 d . . .
Cl1 Cl 0.26943(11) 0.16224(9) 0.84183(8) 0.02969(14) Uani 1 1 d . . .
C1 C 0.2397(3) 0.8097(3) 0.4187(3) 0.0177(4) Uani 1 1 d . . .
N1 N 0.1674(3) 0.6380(3) 0.3034(3) 0.0226(4) Uani 1 1 d . . .
H1 H 0.2301 0.5889 0.2586 0.027 Uiso 1 1 calc R . .
N2 N 0.1156(3) 0.8374(3) 0.4717(3) 0.0203(4) Uani 1 1 d . . .
H2 H 0.1314 0.9452 0.5401 0.024 Uiso 1 1 calc R . .
C2 C -0.0515(3) 0.6662(4) 0.4024(3) 0.0215(5) Uani 1 1 d . . .
H2A H -0.1651 0.6831 0.3623 0.026 Uiso 1 1 calc R . .
H2B H -0.0541 0.6188 0.4844 0.026 Uiso 1 1 calc R . .
C3 C -0.0292(4) 0.5396(4) 0.2593(3) 0.0240(5) Uani 1 1 d . . .
H3A H -0.0588 0.4166 0.2547 0.029 Uiso 1 1 calc R . .
H3B H -0.1081 0.5266 0.1519 0.029 Uiso 1 1 calc R . .
C4 C 0.7644(5) 1.1071(4) 0.9057(4) 0.0371(7) Uani 1 1 d . . .
H4A H 0.7073 1.1885 0.9405 0.056 Uiso 1 1 calc R . .
H4B H 0.8768 1.1756 0.8995 0.056 Uiso 1 1 calc R . .
H4C H 0.7961 1.0602 0.9862 0.056 Uiso 1 1 calc R . .
C5 C 0.7270(5) 0.7806(5) 0.6603(5) 0.0419(8) Uani 1 1 d . . .
H5A H 0.7569 0.7386 0.7449 0.063 Uiso 1 1 calc R . .
H5B H 0.8414 0.8546 0.6602 0.063 Uiso 1 1 calc R . .
H5C H 0.6493 0.6743 0.5516 0.063 Uiso 1 1 calc R . .
C6 C 0.4278(4) 0.7846(4) 0.7465(4) 0.0270(5) Uani 1 1 d . . .
H6A H 0.3412 0.6701 0.6461 0.041 Uiso 1 1 calc R . .
H6B H 0.3611 0.8550 0.7811 0.041 Uiso 1 1 calc R . .
H6C H 0.4855 0.7562 0.8347 0.041 Uiso 1 1 calc R . .
O1 O 0.3879(4) 0.5355(4) 0.1510(4) 0.0450(6) Uani 1 1 d . . .
H1O H 0.354(6) 0.441(7) 0.071(6) 0.047(12) Uiso 1 1 d . . .
H1P H 0.483(7) 0.618(7) 0.155(6) 0.046(12) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01675(7) 0.01193(7) 0.01235(7) 0.00419(5) 0.00815(5) 0.00284(5)
P2 0.0199(3) 0.0162(3) 0.0175(3) 0.0083(2) 0.0103(2) 0.0068(2)
Cl1 0.0412(4) 0.0244(3) 0.0212(3) 0.0089(2) 0.0109(3) 0.0153(3)
C1 0.0208(10) 0.0170(10) 0.0147(10) 0.0078(9) 0.0087(8) 0.0057(9)
N1 0.0241(10) 0.0171(10) 0.0208(10) 0.0044(8) 0.0124(8) 0.0035(8)
N2 0.0194(9) 0.0178(9) 0.0199(10) 0.0059(8) 0.0098(8) 0.0051(8)
C2 0.0183(10) 0.0225(11) 0.0225(11) 0.0112(10) 0.0090(9) 0.0058(9)
C3 0.0224(11) 0.0199(11) 0.0197(11) 0.0064(9) 0.0072(9) 0.0013(9)
C4 0.0430(17) 0.0277(14) 0.0192(12) 0.0100(11) 0.0004(12) 0.0019(13)
C5 0.053(2) 0.0466(19) 0.062(2) 0.0347(18) 0.0420(18) 0.0367(17)
C6 0.0253(12) 0.0335(14) 0.0318(14) 0.0235(12) 0.0160(11) 0.0110(11)
O1 0.0542(16) 0.0300(12) 0.0512(15) 0.0072(11) 0.0389(14) 0.0153(11)
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'
P P 0.1023 0.0942 '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'
Pt Pt -1.7033 8.3905 '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'
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
C1 Pt1 C1 180.00(15) . 2_676 ?
C1 Pt1 P2 90.18(7) . . ?
C1 Pt1 P2 89.82(7) 2_676 . ?
C1 Pt1 P2 89.82(7) . 2_676 ?
C1 Pt1 P2 90.18(7) 2_676 2_676 ?
P2 Pt1 P2 180.0 . 2_676 ?
C5 P2 C6 104.55(16) . . ?
C5 P2 C4 104.17(19) . . ?
C6 P2 C4 103.58(16) . . ?
C5 P2 Pt1 112.61(13) . . ?
C6 P2 Pt1 115.65(9) . . ?
C4 P2 Pt1 114.99(11) . . ?
N2 C1 N1 109.6(2) . . ?
N2 C1 Pt1 125.46(18) . . ?
N1 C1 Pt1 124.93(19) . . ?
C1 N1 C3 112.0(2) . . ?
C1 N2 C2 111.8(2) . . ?
N2 C2 C3 101.6(2) . . ?
N1 C3 C2 101.7(2) . . ?
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
Pt1 C1 2.026(2) . ?
Pt1 C1 2.026(2) 2_676 ?
Pt1 P2 2.3070(6) . ?
Pt1 P2 2.3070(6) 2_676 ?
P2 C5 1.805(3) . ?
P2 C6 1.806(3) . ?
P2 C4 1.805(3) . ?
C1 N2 1.326(3) . ?
C1 N1 1.326(3) . ?
N1 C3 1.466(3) . ?
N2 C2 1.470(3) . ?
C2 C3 1.533(4) . ?
