data_2001818
_journal_name_full 'Acta Crystallographica, Section C'
_journal_year 1993
_journal_volume C49
_journal_page_first 805
_journal_page_last 808
_publ_section_title
;
2-\h^3^-Allyl-1,1,1-tricarbonyl-\m-(\h^1^:\h^6^-diphenyl
methyl)chromiumpalladium(Pd-Cr) at 130 K
;
loop_
_publ_author_name
'Kalinin, Valery N.'
"Cherepanov, Il'ya A."
'Moiseev, Sergey K.'
'Dolgushin, Fedor M.'
'Yanovsky, Alexander I.'
'Struchkov, Yuri T.'
_chemical_name_systematic
;
\h^3^-allylpalladium-\m-(\h^1^:\h^6^-
diphenylmethyl)tricarbonylchromium
;
_chemical_name_common ?
_chemical_formula_moiety 'C19 H16 Cr O3 Pd'
_chemical_formula_sum 'C19 H16 Cr O3 Pd'
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_weight 450.72
_chemical_melting_point ?
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.470(2)
_cell_length_b 12.645(3)
_cell_length_c 13.027(3)
_cell_angle_alpha 118.180(10)
_cell_angle_beta 90.26(2)
_cell_angle_gamma 92.37(2)
_cell_volume 1663.4(6)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 24
_cell_measurement_theta_min 13
_cell_measurement_theta_max 13.5
_cell_measurement_temperature 133.0(10)
_exptl_crystal_description 'well-formed plates'
_exptl_crystal_colour 'light brown'
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_exptl_crystal_density_diffrn 1.800
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 892
_exptl_absorpt_coefficient_mu 1.747
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_diffrn_ambient_temperature 133.0(10)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device 'Siemens P3/PC'
_diffrn_measurement_method '\q/2\q'
_diffrn_reflns_number 7169
_diffrn_reflns_av_R_equivalents 0.0134
_diffrn_reflns_av_sigmaI/netI 0.0227
_diffrn_reflns_theta_min 1.77
_diffrn_reflns_theta_max 27.06
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_standards_number 2
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 1.5
_reflns_number_total 6796
_reflns_number_observed 6032
_reflns_observed_criterion >2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type fullcycle
_refine_ls_R_factor_all 0.0302
_refine_ls_R_factor_obs '0.030 (on F)'
_refine_ls_wR_factor_all 0.0623
_refine_ls_wR_factor_obs '0.063 (on F^2^)'
_refine_ls_goodness_of_fit_all 1.044
_refine_ls_goodness_of_fit_obs 1.063
_refine_ls_restrained_S_all 1.095
_refine_ls_restrained_S_obs 1.063
_refine_ls_number_reflns 6781
_refine_ls_number_parameters 597
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment refall
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.0337P]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_shift/esd_max 0.054
_refine_ls_shift/esd_mean 0.006
_refine_diff_density_max 0.30
_refine_diff_density_min -0.24
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'O' 'O' 0.0106 0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cr' 'Cr' 0.3209 0.6236
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Pd' 'Pd' -0.9988 1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'SHELXTL-PLUS, PC Version (Robinson & Sheldrick, 1988)'
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Pd1_1 0.04823(2) 0.37447(2) 0.70467(2) 0.02118(9) Uani d . 1 . Pd
Cr1_1 0.15534(3) 0.23324(3) 0.49735(3) 0.0200(2) Uani d . 1 . Cr
O1_1 0.1197(2) 0.4866(2) 0.5439(2) 0.0347(11) Uani d . 1 . O
O2_1 0.1205(2) 0.1853(2) 0.2507(2) 0.0486(12) Uani d . 1 . O
O3_1 -0.0957(2) 0.1442(2) 0.4759(2) 0.0404(10) Uani d . 1 . O
C1_1 0.1275(2) 0.3910(2) 0.5330(2) 0.0266(12) Uani d . 1 . C
C2_1 0.1351(2) 0.2029(3) 0.3452(2) 0.0308(13) Uani d . 1 . C
C3_1 -0.0004(2) 0.1832(2) 0.4883(2) 0.0295(14) Uani d . 1 . C
C4_1 -0.0384(3) 0.4923(3) 0.8600(3) 0.034(2) Uani d . 1 . C
H41_1 0.007(4)   0.555(4)   0.914(4)   0.046(12) Uiso d P 0.80 1 H
H42_1 -0.081(3)   0.444(3)   0.885(3)   0.034(10) Uiso d P 0.80 1 H
C5_1 -0.0743(3) 0.5135(4) 0.7671(4) 0.039(2) Uani d P 0.80 1 C
H5_1 -0.052(5)   0.576(5)   0.741(5)   0.085(18) Uiso d P 0.80 1 H
C5'_1 -0.1173(10) 0.4534(11) 0.7675(11) 0.019(5) Uani d P 0.20 2 C
C6_1 -0.1218(4) 0.4264(6) 0.6643(4) 0.039(2) Uani d P 0.80 1 C
H61_1 -0.164(5)   0.364(5)   0.678(5)   0.072(16) Uiso d P 0.80 1 H
H62_1 -0.134(3)   0.441(3)   0.603(3)   0.027(9) Uiso d P 0.80 1 H
C6'_1 -0.0892(14) 0.4801(17) 0.6718(16) 0.028(7) Uani d P 0.20 2 C
C7_1 0.1766(2) 0.3143(2) 0.7825(2) 0.0246(12) Uani d . 1 . C
H7_1 0.226(3)   0.380(3)   0.834(2)   0.026(7) Uiso d . 1 . H
C8_1 0.2261(2) 0.2480(2) 0.6684(2) 0.0216(11) Uani d . 1 . C
C9_1 0.3054(2) 0.3076(2) 0.6245(2) 0.0235(11) Uani d . 1 . C
H9_1 0.325(2)   0.382(3)   0.667(2)   0.023(7) Uiso d . 1 . H
C10_1 0.3501(2) 0.2493(2) 0.5127(2) 0.0268(11) Uani d . 1 . C
H10_1 0.393(3)   0.293(3)   0.490(3)   0.040(9) Uiso d . 1 . H
C11_1 0.3140(2) 0.1292(2) 0.4366(2) 0.0294(13) Uani d . 1 . C
H11_1 0.338(3)   0.091(3)   0.358(3)   0.036(8) Uiso d . 1 . H
C12_1 0.2383(2) 0.0672(2) 0.4761(2) 0.0283(14) Uani d . 1 . C
H12_1 0.215(2)   -0.009(3)   0.428(2)   0.023(7) Uiso d . 1 . H
C13_1 0.1931(2) 0.1254(2) 0.5880(2) 0.0242(12) Uani d . 1 . C
H13_1 0.139(2)   0.082(2)   0.609(2)   0.019(6) Uiso d . 1 . H
C14_1 0.1203(2) 0.2490(2) 0.8412(2) 0.0247(13) Uani d . 1 . C
C15_1 0.1724(3) 0.2562(3) 0.9413(2) 0.032(2) Uani d . 1 . C
H15_1 0.237(3)   0.296(3)   0.967(3)   0.041(9) Uiso d . 1 . H
C16_1 0.1198(3) 0.2009(3) 1.0009(3) 0.043(2) Uani d . 1 . C
H16_1 0.153(3)   0.210(3)   1.066(3)   0.046(9) Uiso d . 1 . H
C17_1 0.0149(3) 0.1370(3) 0.9617(3) 0.042(2) Uani d . 1 . C
H17_1 -0.020(3)   0.106(3)   1.005(3)   0.046(9) Uiso d . 1 . H
C18_1 -0.0385(3) 0.1274(3) 0.8622(3) 0.041(2) Uani d . 1 . C
H18_1 -0.104(3)   0.083(3)   0.831(3)   0.035(9) Uiso d . 1 . H
C19_1 0.0141(3) 0.1825(3) 0.8027(3) 0.0339(14) Uani d . 1 . C
H19_1 -0.022(3)   0.178(3)   0.747(3)   0.050(10) Uiso d . 1 . H
Pd1_2 0.45675(2) 0.63076(2) 0.82447(2) 0.02128(9) Uani d . 1 . Pd
Cr1_2 0.35119(3) 0.78131(3) 0.75591(3) 0.0195(2) Uani d . 1 . Cr
O1_2 0.3853(2) 0.5328(2) 0.5602(2) 0.0363(10) Uani d . 1 . O
O2_2 0.3837(2) 0.8437(2) 0.5621(2) 0.0433(12) Uani d . 1 . O
O3_2 0.6021(2) 0.8692(2) 0.8224(2) 0.0388(10) Uani d . 1 . O
C1_2 0.3784(2) 0.6264(2) 0.6407(2) 0.0268(11) Uani d . 1 . C
C2_2 0.3705(2) 0.8210(2) 0.6370(2) 0.0277(12) Uani d . 1 . C
C3_2 0.5070(2) 0.8303(2) 0.7963(2) 0.0278(14) Uani d . 1 . C
C4_2 0.5461(3) 0.5098(3) 0.8661(3) 0.036(2) Uani d . 1 . C
H41_2 0.586(3)   0.555(3)   0.928(3)   0.024(9) Uiso d P 0.80 1 H
H42_2 0.501(4)   0.447(4)   0.868(4)   0.041(11) Uiso d P 0.80 1 H
C5_2 0.5795(3) 0.4925(4) 0.7549(4) 0.036(2) Uani d P 0.80 1 C
H5_2 0.550(3)   0.421(4)   0.681(4)   0.036(10) Uiso d P 0.80 1 H
C5'_2 0.6203(14) 0.5479(17) 0.8091(13) 0.036(8) Uani d P 0.20 2 C
C6_2 0.6283(4) 0.5842(5) 0.7365(5) 0.034(2) Uani d P 0.80 1 C
H61_2 0.666(4)   0.643(4)   0.793(4)   0.041(12) Uiso d P 0.80 1 H
H62_2 0.644(3)   0.573(3)   0.659(3)   0.014(7) Uiso d P 0.80 1 H
C6'_2 0.5963(14) 0.5338(17) 0.6970(15) 0.028(8) Uani d P 0.20 2 C
C7_2 0.3275(2) 0.6831(2) 0.9548(2) 0.0228(12) Uani d . 1 . C
H7_2 0.281(3)   0.620(3)   0.944(3)   0.032(8) Uiso d . 1 . H
C8_2 0.2793(2) 0.7555(2) 0.9071(2) 0.0201(10) Uani d . 1 . C
C9_2 0.2002(2) 0.7014(2) 0.8073(2) 0.0235(11) Uani d . 1 . C
H9_2 0.179(2)   0.616(3)   0.774(2)   0.023(7) Uiso d . 1 . H
C10_2 0.1569(2) 0.7671(2) 0.7553(2) 0.0271(11) Uani d . 1 . C
H10_2 0.113(3)   0.727(3)   0.690(3)   0.033(8) Uiso d . 1 . H
C11_2 0.1936(2) 0.8881(2) 0.7964(2) 0.0284(13) Uani d . 1 . C
H11_2 0.169(3)   0.930(3)   0.761(3)   0.032(8) Uiso d . 1 . H
C12_2 0.2699(2) 0.9438(2) 0.8937(2) 0.0271(13) Uani d . 1 . C
H12_2 0.294(2)   1.024(3)   0.924(2)   0.025(7) Uiso d . 1 . H
C13_2 0.3142(2) 0.8787(2) 0.9464(2) 0.0234(12) Uani d . 1 . C
H13_2 0.370(2)   0.917(2)   1.009(2)   0.023(7) Uiso d . 1 . H
C14_2 0.3791(2) 0.7448(2) 1.0767(2) 0.0224(12) Uani d . 1 . C
C15_2 0.3169(2) 0.7410(2) 1.1675(2) 0.0271(13) Uani d . 1 . C
H15_2 0.242(3)   0.703(3)   1.151(3)   0.030(7) Uiso d . 1 . H
C16_2 0.3628(3) 0.7954(2) 1.2808(2) 0.032(2) Uani d . 1 . C
H16_2 0.316(3)   0.796(3)   1.340(3)   0.035(8) Uiso d . 1 . H
C17_2 0.4711(3) 0.8547(2) 1.3067(2) 0.030(2) Uani d . 1 . C
H17_2 0.500(3)   0.888(3)   1.383(3)   0.039(8) Uiso d . 1 . H
C18_2 0.5343(2) 0.8599(2) 1.2185(2) 0.0301(14) Uani d . 1 . C
H18_2 0.607(3)   0.898(3)   1.234(3)   0.033(8) Uiso d . 1 . H
C19_2 0.4886(2) 0.8051(2) 1.1048(2) 0.0272(13) Uani d . 1 . C
H19_2 0.536(3)   0.805(3)   1.048(3)   0.037(8) Uiso d . 1 . H