#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:14:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178554 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/62/4066202.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_4066202
loop_
_publ_author_name
'Kessler, Florian'
'Weibert, Bernhard'
'Fischer, Helmut'
_publ_section_title
;
 Bis(allenylidene) Complexes of Palladium and Platinum†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5154
_journal_paper_doi               10.1021/om100346x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C50 H52 N2 O2 P2 Pt, 2(C3 H6 O), 2(B F4)'
_chemical_formula_sum            'C56 H64 B2 F8 N2 O4 P2 Pt'
_chemical_formula_weight         1259.74
_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                 117.76(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.768(3)
_cell_length_b                   15.817(3)
_cell_length_c                   15.353(6)
_cell_measurement_reflns_used    55107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      1.77
_cell_volume                     2743.7(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40405
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  0.6656
_exptl_absorpt_correction_T_min  0.4454
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0204
_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)+(0.0114P)²+2.7464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0418
_reflns_number_gt                5015
_reflns_number_total             5857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100346x_si_001.cif
_cod_data_source_block           fkbw50_&#x0096;_complex_12a-BF4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066202
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
Pt1 Pt 0.5000 0.5000 0.5000 0.01130(3) Uani 1 2 d S
P1 P 0.53567(4) 0.45441(3) 0.65441(4) 0.01199(10) Uani 1 1 d .
O1 O 0.65112(14) 0.19649(10) 0.46934(12) 0.0224(3) Uani 1 1 d .
N1 N 0.80778(17) 0.26896(13) 0.48188(14) 0.0225(4) Uani 1 1 d .
C1 C 0.59047(18) 0.40490(13) 0.48214(14) 0.0145(4) Uani 1 1 d .
F1 F 0.05521(13) 0.24610(11) 0.88429(11) 0.0355(4) Uani 1 1 d .
B1 B 0.1168(2) 0.27051(18) 0.8333(2) 0.0250(5) Uani 1 1 d .
C2 C 0.64254(19) 0.34700(14) 0.47076(16) 0.0183(4) Uani 1 1 d .
F2 F 0.05105(15) 0.25158(13) 0.73418(11) 0.0472(4) Uani 1 1 d .
O2 O 0.13131(16) 0.56153(12) 0.83794(15) 0.0353(4) Uani 1 1 d .
C3 C 0.70123(19) 0.27038(14) 0.47360(15) 0.0174(4) Uani 1 1 d .
F3 F 0.13888(19) 0.35615(11) 0.84591(14) 0.0523(5) Uani 1 1 d .
C4 C 0.8705(2) 0.34698(18) 0.4842(2) 0.0340(6) Uani 1 1 d .
H4A H 0.8191 0.3956 0.4759 0.051 Uiso 1 1 calc R
H4B H 0.8921 0.3462 0.4307 0.051 Uiso 1 1 calc R
H4C H 0.9423 0.3514 0.5475 0.051 Uiso 1 1 calc R
F4 F 0.22355(16) 0.22819(13) 0.87168(14) 0.0545(5) Uani 1 1 d .
C5 C 0.8735(2) 0.18970(18) 0.4930(2) 0.0338(6) Uani 1 1 d .
H5A H 0.8236 0.1416 0.4900 0.051 Uiso 1 1 calc R
H5B H 0.9453 0.1897 0.5566 0.051 Uiso 1 1 calc R
H5C H 0.8952 0.1851 0.4398 0.051 Uiso 1 1 calc R
C6 C 0.5350(2) 0.19577(16) 0.4677(2) 0.0305(6) Uani 1 1 d .
H6A H 0.4717 0.2111 0.4015 0.037 Uiso 1 1 calc R
H6B H 0.5339 0.2366 0.5161 0.037 Uiso 1 1 calc R
C7 C 0.5169(3) 0.10749(17) 0.4939(2) 0.0395(7) Uani 1 1 d .
H7A H 0.4402 0.1038 0.4937 0.059 Uiso 1 1 calc R
H7B H 0.5802 0.0932 0.5595 0.059 Uiso 1 1 calc R
H7C H 0.5185 0.0678 0.4455 0.059 Uiso 1 1 calc R
C21 C 0.62788(17) 0.52522(13) 0.75341(15) 0.0144(4) Uani 1 1 d .
C22 C 0.65855(18) 0.60488(14) 0.73311(16) 0.0172(4) Uani 1 1 d .
H22A H 0.6348 0.6212 0.6670 0.021 Uiso 1 1 calc R
C23 C 0.7239(2) 0.66036(15) 0.80979(17) 0.0224(5) Uani 1 1 d .
H23A H 0.7452 0.7144 0.7959 0.027 Uiso 1 1 calc R
C24 C 0.7580(2) 0.63697(16) 0.90634(17) 0.0241(5) Uani 1 1 d .
H24A H 0.8002 0.6757 0.9583 0.029 Uiso 1 1 calc R
C25 C 0.73046(19) 0.55689(15) 0.92721(16) 0.0214(5) Uani 1 1 d .
H25A H 0.7551 0.5406 0.9935 0.026 Uiso 1 1 calc R
C26 C 0.66707(16) 0.50095(17) 0.85126(14) 0.0183(4) Uani 1 1 d .
H26A H 0.6501 0.4458 0.8657 0.022 Uiso 1 1 calc R
C31 C 0.39575(17) 0.44287(13) 0.65683(15) 0.0142(4) Uani 1 1 d .
C32 C 0.37877(19) 0.46825(14) 0.73609(16) 0.0182(4) Uani 1 1 d .
H32A H 0.4392 0.4986 0.7890 0.022 Uiso 1 1 calc R
C33 C 0.2736(2) 0.44932(16) 0.73812(17) 0.0242(5) Uani 1 1 d .
H33A H 0.2624 0.4664 0.7925 0.029 Uiso 1 1 calc R
C34 C 0.1854(2) 0.40549(16) 0.66065(18) 0.0261(5) Uani 1 1 d .
H34A H 0.1142 0.3914 0.6627 0.031 Uiso 1 1 calc R
C35 C 0.2003(2) 0.38195(16) 0.57993(18) 0.0244(5) Uani 1 1 d .
H35A H 0.1388 0.3529 0.5264 0.029 Uiso 1 1 calc R
C36 C 0.30483(19) 0.40081(15) 0.57756(16) 0.0197(4) Uani 1 1 d .
H36A H 0.3148 0.3852 0.5221 0.024 Uiso 1 1 calc R
C41 C 0.60483(18) 0.35126(13) 0.69270(15) 0.0152(4) Uani 1 1 d .
C42 C 0.5463(2) 0.28240(14) 0.70702(16) 0.0193(4) Uani 1 1 d .
H42A H 0.4695 0.2896 0.7015 0.023 Uiso 1 1 calc R
C43 C 0.6000(2) 0.20333(15) 0.72937(17) 0.0243(5) Uani 1 1 d .
H43A H 0.5599 0.1567 0.7395 0.029 Uiso 1 1 calc R
C44 C 0.7114(2) 0.19208(15) 0.73702(17) 0.0267(5) Uani 1 1 d .
H44A H 0.7469 0.1376 0.7507 0.032 Uiso 1 1 calc R
C45 C 0.7715(2) 0.26053(16) 0.72461(17) 0.0247(5) Uani 1 1 d .
H45A H 0.8486 0.2531 0.7310 0.030 Uiso 1 1 calc R
C46 C 0.71855(19) 0.33977(15) 0.70280(16) 0.0200(4) Uani 1 1 d .
H46A H 0.7599 0.3865 0.6947 0.024 Uiso 1 1 calc R
C100 C 0.0305(2) 0.53514(16) 0.80021(19) 0.0264(5) Uani 1 1 d .
C101 C -0.0253(2) 0.5021(2) 0.86041(18) 0.0334(5) Uani 1 1 d .
H10A H 0.0319 0.5053 0.9304 0.050 Uiso 1 1 calc R
H10B H -0.0492 0.4432 0.8425 0.050 Uiso 1 1 calc R
H10C H -0.0950 0.5363 0.8477 0.050 Uiso 1 1 calc R
C102 C -0.0458(3) 0.5340(2) 0.6908(2) 0.0427(7) Uani 1 1 d .
H10D H -0.0016 0.5575 0.6587 0.064 Uiso 1 1 calc R
H10E H -0.1169 0.5680 0.6736 0.064 Uiso 1 1 calc R
H10F H -0.0687 0.4756 0.6687 0.064 Uiso 1 1 calc R
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
C1 Pt1 C1 180.000(1) 3_666 .
C1 Pt1 P1 86.80(6) 3_666 .
C1 Pt1 P1 93.20(6) . .
C1 Pt1 P1 93.20(6) 3_666 3_666
C1 Pt1 P1 86.80(6) . 3_666
P1 Pt1 P1 180.000(10) . 3_666
C21 P1 C31 107.84(10) . .
C21 P1 C41 104.81(10) . .
C31 P1 C41 103.77(10) . .
C21 P1 Pt1 114.08(7) . .
C31 P1 Pt1 109.09(7) . .
C41 P1 Pt1 116.47(7) . .
C3 O1 C6 117.99(17) . .
C3 N1 C4 121.4(2) . .
C3 N1 C5 122.5(2) . .
C4 N1 C5 116.1(2) . .
C2 C1 Pt1 178.64(18) . .
F3 B1 F4 108.6(2) . .
F3 B1 F2 110.2(2) . .
F4 B1 F2 109.7(2) . .
F3 B1 F1 108.9(2) . .
F4 B1 F1 109.2(2) . .
F2 B1 F1 110.2(2) . .
C1 C2 C3 167.9(2) . .
N1 C3 O1 116.7(2) . .
N1 C3 C2 122.0(2) . .
O1 C3 C2 121.31(19) . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 H5A 109.5 . .
N1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
N1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O1 C6 C7 106.4(2) . .
O1 C6 H6A 110.5 . .
C7 C6 H6A 110.5 . .
O1 C6 H6B 110.5 . .
C7 C6 H6B 110.5 . .
H6A C6 H6B 108.6 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C22 C21 C26 119.4(2) . .
C22 C21 P1 120.69(16) . .
C26 C21 P1 119.94(17) . .
C23 C22 C21 120.0(2) . .
C23 C22 H22A 120.0 . .
C21 C22 H22A 120.0 . .
C24 C23 C22 120.1(2) . .
C24 C23 H23A 119.9 . .
C22 C23 H23A 119.9 . .
C23 C24 C25 120.1(2) . .
C23 C24 H24A 119.9 . .
C25 C24 H24A 119.9 . .
C26 C25 C24 119.9(2) . .
C26 C25 H25A 120.0 . .
C24 C25 H25A 120.0 . .
C25 C26 C21 120.4(2) . .
C25 C26 H26A 119.8 . .
C21 C26 H26A 119.8 . .
C32 C31 C36 119.62(19) . .
C32 C31 P1 123.05(16) . .
C36 C31 P1 117.16(16) . .
C33 C32 C31 120.2(2) . .
C33 C32 H32A 119.9 . .
C31 C32 H32A 119.9 . .
C34 C33 C32 119.8(2) . .
C34 C33 H33A 120.1 . .
C32 C33 H33A 120.1 . .
C33 C34 C35 120.4(2) . .
C33 C34 H34A 119.8 . .
C35 C34 H34A 119.8 . .
C36 C35 C34 120.0(2) . .
C36 C35 H35A 120.0 . .
C34 C35 H35A 120.0 . .
C35 C36 C31 120.0(2) . .
C35 C36 H36A 120.0 . .
C31 C36 H36A 120.0 . .
C42 C41 C46 119.1(2) . .
C42 C41 P1 122.43(16) . .
C46 C41 P1 118.39(16) . .
C43 C42 C41 120.1(2) . .
C43 C42 H42A 119.9 . .
C41 C42 H42A 119.9 . .
C44 C43 C42 120.4(2) . .
C44 C43 H43A 119.8 . .
C42 C43 H43A 119.8 . .
C43 C44 C45 120.0(2) . .
C43 C44 H44A 120.0 . .
C45 C44 H44A 120.0 . .
C46 C45 C44 119.9(2) . .
C46 C45 H45A 120.1 . .
C44 C45 H45A 120.1 . .
C45 C46 C41 120.5(2) . .
C45 C46 H46A 119.7 . .
C41 C46 H46A 119.7 . .
O2 C100 C102 122.1(2) . .
O2 C100 C101 121.9(2) . .
C102 C100 C101 116.0(2) . .
C100 C101 H10A 109.5 . .
C100 C101 H10B 109.5 . .
H10A C101 H10B 109.5 . .
C100 C101 H10C 109.5 . .
H10A C101 H10C 109.5 . .
H10B C101 H10C 109.5 . .
C100 C102 H10D 109.5 . .
C100 C102 H10E 109.5 . .
H10D C102 H10E 109.5 . .
C100 C102 H10F 109.5 . .
H10D C102 H10F 109.5 . .
H10E C102 H10F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C1 1.992(2) 3_666
Pt1 C1 1.992(2) .
Pt1 P1 2.3113(10) .
Pt1 P1 2.3113(10) 3_666
P1 C21 1.812(2) .
P1 C31 1.813(2) .
P1 C41 1.818(2) .
O1 C3 1.319(3) .
O1 C6 1.471(3) .
N1 C3 1.306(3) .
N1 C4 1.462(3) .
N1 C5 1.473(3) .
C1 C2 1.191(3) .
F1 B1 1.398(3) .
B1 F3 1.379(3) .
B1 F4 1.380(3) .
B1 F2 1.386(3) .
C2 C3 1.415(3) .
O2 C100 1.213(3) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.500(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C21 C22 1.397(3) .
C21 C26 1.398(3) .
C22 C23 1.392(3) .
C22 H22A 0.9500 .
C23 C24 1.387(3) .
C23 H23A 0.9500 .
C24 C25 1.391(3) .
C24 H24A 0.9500 .
C25 C26 1.385(3) .
C25 H25A 0.9500 .
C26 H26A 0.9500 .
C31 C32 1.391(3) .
C31 C36 1.398(3) .
C32 C33 1.390(3) .
C32 H32A 0.9500 .
C33 C34 1.384(3) .
C33 H33A 0.9500 .
C34 C35 1.389(3) .
C34 H34A 0.9500 .
C35 C36 1.385(3) .
C35 H35A 0.9500 .
C36 H36A 0.9500 .
C41 C42 1.395(3) .
C41 C46 1.398(3) .
C42 C43 1.390(3) .
C42 H42A 0.9500 .
C43 C44 1.384(3) .
C43 H43A 0.9500 .
C44 C45 1.390(4) .
C44 H44A 0.9500 .
C45 C46 1.389(3) .
C45 H45A 0.9500 .
C46 H46A 0.9500 .
C100 C102 1.498(4) .
C100 C101 1.499(3) .
C101 H10A 0.9800 .
C101 H10B 0.9800 .
C101 H10C 0.9800 .
C102 H10D 0.9800 .
C102 H10E 0.9800 .
C102 H10F 0.9800 .
