#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:45:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178666 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/77/4077729.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_4077729
loop_
_publ_author_name
'Ruiz, José'
'Rodríguez, Venancio'
'López, Gregorio'
'Casabó, Jaume'
'Molins, Elies'
'Miravitlles, Carles'
_publ_section_title
;
 Reactivity of [{M(C6F5)2(μ-OH)}2]2-(M = Pd or Pt) toward Aromatic Amines
 and Malononitrile
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1177
_journal_paper_doi               10.1021/om980508z
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C34 H37 F15 N2 Pd'
_chemical_formula_weight         865.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 97.88(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   12.567(3)
_cell_length_b                   17.637(6)
_cell_length_c                   17.016(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3735.9(18)
_computing_data_reduction        MolEN
_computing_publication_material  CIFDAT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6793
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        -1.2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.9872
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.234
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.216
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_obs          0.0642
_refine_ls_shift/esd_max         2.561
_refine_ls_shift/esd_mean        0.108
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1158P)²+2.8094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2425
_refine_ls_wR_factor_obs         0.1751
_reflns_number_observed          2888
_reflns_number_total             6558
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980508z.cif
_cod_data_source_block           um5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'PSI scan' changed to
'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+2.8094P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+2.8094P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4077729
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.52423(5) 0.08723(3) 0.49441(4) 0.0817(3) Uani 1 d .
F3 F 0.2056(4) 0.0314(4) 0.3543(5) 0.142(2) Uani 1 d D
F4 F 0.1646(6) 0.0226(4) 0.1953(6) 0.176(3) Uani 1 d D
F5 F 0.3268(7) -0.0082(4) 0.1123(5) 0.173(3) Uani 1 d D
F6 F 0.5276(6) -0.0318(5) 0.1873(4) 0.152(3) Uani 1 d D
F7 F 0.5674(4) -0.0232(3) 0.3458(3) 0.111(2) Uani 1 d D
F9 F 0.7719(5) 0.1113(4) 0.4911(4) 0.133(2) Uani 1 d D
F10 F 0.9104(5) 0.2094(5) 0.5635(5) 0.175(3) Uani 1 d D
F11 F 0.8467(6) 0.3138(4) 0.6690(4) 0.148(2) Uani 1 d D
F12 F 0.6413(6) 0.3114(5) 0.6982(5) 0.169(3) Uani 1 d D
F13 F 0.5006(5) 0.2138(4) 0.6243(5) 0.163(3) Uani 1 d D
F15 F 0.6078(5) 0.1617(4) 0.3483(4) 0.143(2) Uani 1 d D
F16 F 0.5443(7) 0.2818(5) 0.2578(4) 0.179(3) Uani 1 d D
F17 F 0.3676(9) 0.3583(4) 0.2797(5) 0.205(4) Uani 1 d D
F18 F 0.2551(10) 0.3134(7) 0.3969(7) 0.282(7) Uani 1 d D
F19 F 0.3165(6) 0.1944(6) 0.4893(5) 0.197(4) Uani 1 d D
N1 N 0.4229(7) 0.0171(5) 0.4365(5) 0.119(4) Uani 1 d .
H1 H 0.3606(7) 0.0289(5) 0.4554(5) 0.072(22) Uiso 1 calc R
C2 C 0.3891(7) 0.0032(4) 0.3608(8) 0.112(5) Uani 1 d D
C3 C 0.2904(8) 0.0147(5) 0.3166(7) 0.102(3) Uani 1 d D
C4 C 0.2646(8) 0.0117(6) 0.2367(9) 0.121(4) Uani 1 d D
C5 C 0.3447(11) -0.0054(6) 0.1928(6) 0.127(5) Uani 1 d D
C6 C 0.4464(9) -0.0155(6) 0.2296(7) 0.099(3) Uani 1 d D
C7 C 0.4645(6) -0.0105(5) 0.3103(6) 0.092(3) Uani 1 d D
C8 C 0.6300(6) 0.1596(5) 0.5528(5) 0.084(2) Uani 1 d D
C9 C 0.7359(6) 0.1615(5) 0.5416(5) 0.090(3) Uani 1 d D
C10 C 0.8081(6) 0.2107(6) 0.5796(6) 0.107(3) Uani 1 d D
C11 C 0.7778(8) 0.2620(5) 0.6322(6) 0.102(3) Uani 1 d D
C12 C 0.6742(8) 0.2604(5) 0.6467(6) 0.103(3) Uani 1 d D
C13 C 0.6033(6) 0.2107(5) 0.6075(6) 0.100(3) Uani 1 d D
C14 C 0.4677(7) 0.1747(4) 0.4240(5) 0.084(2) Uani 1 d D
C15 C 0.5183(7) 0.1982(5) 0.3626(5) 0.093(3) Uani 1 d D
C16 C 0.4890(9) 0.2580(6) 0.3155(6) 0.111(3) Uani 1 d D
C17 C 0.4008(11) 0.2982(6) 0.3256(7) 0.137(5) Uani 1 d D
C18 C 0.3452(9) 0.2754(7) 0.3845(8) 0.149(5) Uani 1 d D
C19 C 0.3760(8) 0.2147(6) 0.4316(6) 0.121(4) Uani 1 d D
N2 N 0.8369(6) 0.0765(4) 0.2260(5) 0.093(2) Uani 1 d U
C20 C 0.7280(8) 0.1050(6) 0.1842(6) 0.108(3) Uani 1 d D
H201 H 0.6834(8) 0.0613(6) 0.1681(6) 0.230(13) Uiso 1 calc R
H202 H 0.6931(8) 0.1331(6) 0.2225(6) 0.230(13) Uiso 1 calc R
C21 C 0.7316(10) 0.1538(7) 0.1136(8) 0.136(4) Uani 1 d D
H211 H 0.7748(10) 0.1984(7) 0.1286(8) 0.230(13) Uiso 1 calc R
H212 H 0.7648(10) 0.1263(7) 0.0740(8) 0.230(13) Uiso 1 calc R
C22 C 0.6215(13) 0.1774(8) 0.0793(10) 0.171(6) Uani 1 d D
H221 H 0.5862(13) 0.2004(8) 0.1207(10) 0.230(13) Uiso 1 calc R
H222 H 0.6264(13) 0.2155(8) 0.0389(10) 0.230(13) Uiso 1 calc R
C23 C 0.5557(13) 0.1141(10) 0.0443(11) 0.206(8) Uani 1 d D
H231 H 0.5982(31) 0.0824(39) 0.0149(58) 0.230(13) Uiso 1 calc R
H232 H 0.4954(55) 0.1335(10) 0.0094(57) 0.230(13) Uiso 1 calc R
H233 H 0.5305(79) 0.0850(41) 0.0857(12) 0.230(13) Uiso 1 calc R
C24 C 0.9075(9) 0.1422(7) 0.2570(7) 0.127(4) Uani 1 d D
H241 H 0.9765(9) 0.1221(7) 0.2804(7) 0.230(13) Uiso 1 calc R
H242 H 0.9199(9) 0.1735(7) 0.2123(7) 0.230(13) Uiso 1 calc R
C25 C 0.8652(12) 0.1916(8) 0.3171(9) 0.183(7) Uani 1 d D
H251 H 0.8568(12) 0.1621(8) 0.3640(9) 0.230(13) Uiso 1 calc R
H252 H 0.7953(12) 0.2114(8) 0.2954(9) 0.230(13) Uiso 1 calc R
C26 C 0.9434(16) 0.2574(11) 0.3396(12) 0.274(14) Uani 1 d D
H261 H 1.0011(16) 0.2418(11) 0.3802(12) 0.230(13) Uiso 1 calc R
H262 H 0.9742(16) 0.2750(11) 0.2937(12) 0.230(13) Uiso 1 calc R
C27 C 0.8776(28) 0.3179(15) 0.3700(25) 0.795(43) Uiso 1 d D
H271 H 0.8596(82) 0.3034(33) 0.4209(40) 0.230(13) Uiso 1 calc R
H272 H 0.8129(52) 0.3251(48) 0.3336(42) 0.230(13) Uiso 1 calc R
H273 H 0.9177(45) 0.3644(23) 0.3750(69) 0.230(13) Uiso 1 calc R
C28 C 0.8098(9) 0.0239(6) 0.2922(7) 0.111(3) Uani 1 d D
H281 H 0.7710(9) 0.0534(6) 0.3271(7) 0.230(13) Uiso 1 calc R
H282 H 0.7612(9) -0.0149(6) 0.2681(7) 0.230(13) Uiso 1 calc R
C29 C 0.9021(12) -0.0152(9) 0.3428(9) 0.182(6) Uani 1 d D
H291 H 0.9455(12) 0.0211(9) 0.3759(9) 0.230(13) Uiso 1 calc R
H292 H 0.9474(12) -0.0416(9) 0.3099(9) 0.230(13) Uiso 1 calc R
C30 C 0.8451(15) -0.0748(12) 0.3968(11) 0.264(12) Uani 1 d D
H301 H 0.7763(15) -0.0550(12) 0.4072(11) 0.230(13) Uiso 1 calc R
H302 H 0.8329(15) -0.1228(12) 0.3693(11) 0.230(13) Uiso 1 calc R
C31 C 0.9138(28) -0.0850(19) 0.4685(13) 0.531(31) Uiso 1 d D
H311 H 0.8809(51) -0.1190(57) 0.5020(32) 0.230(13) Uiso 1 calc R
H312 H 0.9265(83) -0.0370(21) 0.4947(38) 0.230(13) Uiso 1 calc R
H313 H 0.9808(45) -0.1059(68) 0.4577(14) 0.230(13) Uiso 1 calc R
C32 C 0.8980(8) 0.0367(7) 0.1697(7) 0.120(4) Uani 1 d D
H321 H 0.9132(8) 0.0722(7) 0.1292(7) 0.230(13) Uiso 1 calc R
H322 H 0.9662(8) 0.0199(7) 0.1981(7) 0.230(13) Uiso 1 calc R
C33 C 0.8391(12) -0.0317(8) 0.1296(8) 0.164(6) Uani 1 d D
H331 H 0.7673(12) -0.0180(8) 0.1054(8) 0.230(13) Uiso 1 calc R
H332 H 0.8341(12) -0.0723(8) 0.1674(8) 0.230(13) Uiso 1 calc R
C34 C 0.9093(17) -0.0553(10) 0.0663(11) 0.256(12) Uani 1 d D
H341 H 0.9167(17) -0.0130(10) 0.0311(11) 0.230(13) Uiso 1 calc R
H342 H 0.9803(17) -0.0694(10) 0.0918(11) 0.230(13) Uiso 1 calc R
C35 C 0.8603(19) -0.1193(12) 0.0206(12) 0.288(12) Uiso 1 d D
H351 H 0.8214(81) -0.1012(13) -0.0283(34) 0.230(13) Uiso 1 calc R
H352 H 0.8120(72) -0.1450(41) 0.0506(31) 0.230(13) Uiso 1 calc R
H353 H 0.9154(19) -0.1537(35) 0.0093(60) 0.230(13) Uiso 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
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'
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
N1 Pd1 C8 179.1(4) . .
N1 Pd1 C14 91.9(4) . .
C8 Pd1 C14 87.9(4) . .
N1 Pd1 N1 82.5(3) . 3_656
C8 Pd1 N1 97.7(3) . 3_656
C14 Pd1 N1 174.3(3) . 3_656
N1 Pd1 Pd1 44.8(2) . 3_656
C8 Pd1 Pd1 135.5(3) . 3_656
C14 Pd1 Pd1 136.6(3) . 3_656
N1 Pd1 Pd1 37.8(2) 3_656 3_656
C2 N1 Pd1 135.4(8) . .
C2 N1 Pd1 113.1(6) . 3_656
Pd1 N1 Pd1 97.5(3) . 3_656
N1 C2 C3 130.5(10) . .
N1 C2 C7 118.8(9) . .
C3 C2 C7 109.2(10) . .
C4 C3 F3 112.9(10) . .
C4 C3 C2 128.1(9) . .
F3 C3 C2 119.0(10) . .
C3 C4 C5 117.6(8) . .
C3 C4 F4 126.0(12) . .
C5 C4 F4 116.3(12) . .
F5 C5 C6 118.4(12) . .
F5 C5 C4 121.8(12) . .
C6 C5 C4 119.7(9) . .
F6 C6 C5 120.9(11) . .
F6 C6 C7 120.9(10) . .
C5 C6 C7 118.2(8) . .
F7 C7 C6 116.8(9) . .
F7 C7 C2 116.1(9) . .
C6 C7 C2 127.1(8) . .
C13 C8 C9 114.3(7) . .
C13 C8 Pd1 123.2(6) . .
C9 C8 Pd1 122.5(6) . .
C10 C9 F9 117.5(7) . .
C10 C9 C8 123.3(7) . .
F9 C9 C8 119.2(7) . .
F10 C10 C9 119.2(8) . .
F10 C10 C11 120.2(8) . .
C9 C10 C11 120.6(7) . .
F11 C11 C12 119.9(9) . .
F11 C11 C10 122.3(9) . .
C12 C11 C10 117.7(7) . .
F12 C12 C13 120.5(8) . .
F12 C12 C11 119.1(8) . .
C13 C12 C11 120.4(7) . .
C12 C13 F13 116.7(7) . .
C12 C13 C8 123.5(7) . .
F13 C13 C8 119.8(7) . .
C15 C14 C19 113.7(8) . .
C15 C14 Pd1 121.6(6) . .
C19 C14 Pd1 124.7(6) . .
C16 C15 F15 115.8(8) . .
C16 C15 C14 125.3(8) . .
F15 C15 C14 118.9(8) . .
C15 C16 F16 123.5(10) . .
C15 C16 C17 120.0(8) . .
F16 C16 C17 116.5(10) . .
F17 C17 C16 122.3(11) . .
F17 C17 C18 120.7(12) . .
C16 C17 C18 117.0(8) . .
F18 C18 C17 119.6(11) . .
F18 C18 C19 118.2(11) . .
C17 C18 C19 122.2(8) . .
C18 C19 F19 119.4(9) . .
C18 C19 C14 121.6(8) . .
F19 C19 C14 118.9(8) . .
C32 N2 C24 104.9(7) . .
C32 N2 C28 112.0(9) . .
C24 N2 C28 112.7(8) . .
C32 N2 C20 111.3(8) . .
C24 N2 C20 110.7(8) . .
C28 N2 C20 105.4(7) . .
C21 C20 N2 116.2(9) . .
C22 C21 C20 110.5(10) . .
C23 C22 C21 112.9(12) . .
C25 C24 N2 116.1(9) . .
C24 C25 C26 109.6(11) . .
C27 C26 C25 105.2(16) . .
C29 C28 N2 117.7(10) . .
C28 C29 C30 104.7(11) . .
C31 C30 C29 107.9(16) . .
C33 C32 N2 113.6(9) . .
C32 C33 C34 103.7(11) . .
C35 C34 C33 110.0(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 1.944(9) .
Pd1 C8 2.006(8) .
Pd1 C14 2.021(8) .
Pd1 N1 2.235(9) 3_656
Pd1 Pd1 3.147(2) 3_656
F3 C3 1.349(7) .
F4 C4 1.367(8) .
F5 C5 1.359(8) .
F6 C6 1.356(7) .
F7 C7 1.368(7) .
F9 C9 1.355(7) .
F10 C10 1.351(7) .
F11 C11 1.352(7) .
F12 C12 1.359(7) .
F13 C13 1.360(7) .
F15 C15 1.347(7) .
F16 C16 1.346(8) .
F17 C17 1.347(8) .
F18 C18 1.357(8) .
F19 C19 1.363(7) .
N1 C2 1.323(13) .
N1 Pd1 2.235(9) 3_656
C2 C3 1.375(9) .
C2 C7 1.384(9) .
C3 C4 1.354(9) .
C4 C5 1.367(9) .
C5 C6 1.356(9) .
C6 C7 1.364(9) .
C8 C13 1.371(8) .
C8 C9 1.369(8) .
C9 C10 1.354(8) .
C10 C11 1.364(9) .
C11 C12 1.359(9) .
C12 C13 1.357(8) .
C14 C15 1.361(8) .
C14 C19 1.372(8) .
C15 C16 1.345(9) .
C16 C17 1.347(9) .
C17 C18 1.358(9) .
C18 C19 1.362(9) .
N2 C32 1.484(11) .
N2 C24 1.510(12) .
N2 C28 1.532(12) .
N2 C20 1.538(12) .
C20 C21 1.484(12) .
C21 C22 1.485(13) .
C22 C23 1.466(14) .
C24 C25 1.496(13) .
C25 C26 1.535(14) .
C26 C27 1.49(2) .
C28 C29 1.513(13) .
C29 C30 1.62(2) .
C30 C31 1.41(2) .
C32 C33 1.526(13) .
C33 C34 1.54(2) .
C34 C35 1.46(2) .
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
N2 C20 C21 C22 -179.9(10)
C20 C21 C22 C23 -67.7(19)
N2 C24 C25 C26 -177.4(14)
C24 C25 C26 C27 156.8(24)
N2 C28 C29 C30 -171.9(12)
C28 C29 C30 C31 -151.1(23)
N2 C32 C33 C34 171.8(12)
C32 C33 C34 C35 -177.9(16)
