#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:37:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179509 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/06/4340659.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_4340659
loop_
_publ_author_name
'Comanescu, Cezar C.'
'Iluc, Vlad M.'
_publ_section_title
;
 Flexible Coordination of Diphosphine Ligands Leading to cis and trans
 Pd(0), Pd(II), and Rh(I) Complexes.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8517
_journal_page_last               8528
_journal_paper_doi               10.1021/ic5010566
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C26 H40 P2'
_chemical_formula_weight         414.52
_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                88.779(2)
_cell_angle_beta                 78.166(2)
_cell_angle_gamma                72.008(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1305(9)
_cell_length_b                   7.2635(9)
_cell_length_c                   12.7304(17)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.484
_cell_measurement_theta_min      2.389
_cell_volume                     613.14(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'combination of ω- and φ-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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12575
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             226
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0271
_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)+(0.0335P)²+0.2544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                2056
_reflns_number_total             2158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5010566_si_002.cif
_cod_data_source_block           cc04
_cod_depositor_comments
'Adding full bibliography for 4340659--4340669.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340659
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
C1 C -0.07758(18) 0.94753(17) 0.99648(9) 0.0159(3) Uani 1 1 d .
H1A H -0.0059 0.8108 0.9718 0.019 Uiso 1 1 calc R
H1B H -0.1623 0.9486 1.0687 0.019 Uiso 1 1 calc R
P1 P 0.08034(4) 0.80235(4) 0.75412(2) 0.01359(11) Uani 1 1 d .
C14 C -0.45877(19) 1.25213(18) 0.78489(11) 0.0220(3) Uani 1 1 d .
H14 H -0.5421 1.3229 0.7388 0.026 Uiso 1 1 calc R
C31 C 0.15514(19) 0.87841(17) 0.61527(10) 0.0177(3) Uani 1 1 d .
H31 H 0.0381 0.9081 0.5789 0.021 Uiso 1 1 calc R
C32 C -0.01142(19) 0.59454(17) 0.73141(10) 0.0178(3) Uani 1 1 d .
H32 H 0.1089 0.4885 0.6935 0.021 Uiso 1 1 calc R
C33 C 0.2192(2) 1.0594(2) 0.62132(12) 0.0285(3) Uani 1 1 d .
H33A H 0.2654 1.0967 0.5485 0.043 Uiso 1 1 calc R
H33B H 0.3292 1.0322 0.6604 0.043 Uiso 1 1 calc R
H33C H 0.1043 1.1656 0.6590 0.043 Uiso 1 1 calc R
C34 C 0.3298(2) 0.71227(19) 0.55301(10) 0.0240(3) Uani 1 1 d .
H34A H 0.3839 0.7568 0.4835 0.036 Uiso 1 1 calc R
H34B H 0.2812 0.6036 0.5412 0.036 Uiso 1 1 calc R
H34C H 0.4362 0.6700 0.5944 0.036 Uiso 1 1 calc R
C35 C -0.1691(2) 0.6291(2) 0.66241(12) 0.0290(3) Uani 1 1 d .
H35A H -0.1998 0.5086 0.6533 0.044 Uiso 1 1 calc R
H35B H -0.1169 0.6714 0.5919 0.044 Uiso 1 1 calc R
H35C H -0.2922 0.7296 0.6977 0.044 Uiso 1 1 calc R
C36 C -0.0845(2) 0.51859(19) 0.84013(11) 0.0245(3) Uani 1 1 d .
H36A H -0.1201 0.4016 0.8287 0.037 Uiso 1 1 calc R
H36B H -0.2033 0.6180 0.8803 0.037 Uiso 1 1 calc R
H36C H 0.0229 0.4875 0.8810 0.037 Uiso 1 1 calc R
C16 C -0.38738(19) 1.19383(18) 0.96067(10) 0.0198(3) Uani 1 1 d .
H16 H -0.4242 1.2250 1.0357 0.024 Uiso 1 1 calc R
C15 C -0.51032(19) 1.29805(18) 0.89432(11) 0.0225(3) Uani 1 1 d .
H15 H -0.6292 1.4003 0.9237 0.027 Uiso 1 1 calc R
C13 C -0.28514(19) 1.10244(18) 0.74299(10) 0.0188(3) Uani 1 1 d .
H13 H -0.2517 1.0709 0.6680 0.023 Uiso 1 1 calc R
C12 C -0.15752(18) 0.99634(17) 0.80850(10) 0.0148(3) Uani 1 1 d .
C11 C -0.21053(18) 1.04408(17) 0.91977(10) 0.0153(3) Uani 1 1 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'
P P 0.1023 0.0942 '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
C11 C1 C1 111.10(12) . 2_577
C11 C1 H1A 109.4 . .
C1 C1 H1A 109.4 2_577 .
C11 C1 H1B 109.4 . .
C1 C1 H1B 109.4 2_577 .
H1A C1 H1B 108.0 . .
C12 P1 C31 102.76(5) . .
C12 P1 C32 102.25(6) . .
C31 P1 C32 102.83(6) . .
C15 C14 C13 119.70(12) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C33 C31 C34 110.57(11) . .
C33 C31 P1 108.93(9) . .
C34 C31 P1 108.62(8) . .
C33 C31 H31 109.6 . .
C34 C31 H31 109.6 . .
P1 C31 H31 109.6 . .
C35 C32 C36 110.71(11) . .
C35 C32 P1 117.05(9) . .
C36 C32 P1 109.02(9) . .
C35 C32 H32 106.5 . .
C36 C32 H32 106.5 . .
P1 C32 H32 106.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C31 C34 H34A 109.5 . .
C31 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C31 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C32 C35 H35A 109.5 . .
C32 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C32 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C32 C36 H36A 109.5 . .
C32 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C32 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C15 C16 C11 121.55(12) . .
C15 C16 H16 119.2 . .
C11 C16 H16 119.2 . .
C14 C15 C16 119.58(12) . .
C14 C15 H15 120.2 . .
C16 C15 H15 120.2 . .
C14 C13 C12 121.66(12) . .
C14 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
C13 C12 C11 118.36(11) . .
C13 C12 P1 122.62(9) . .
C11 C12 P1 118.99(9) . .
C16 C11 C12 119.13(11) . .
C16 C11 C1 118.10(11) . .
C12 C11 C1 122.68(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C11 1.5113(17) .
C1 C1 1.542(2) 2_577
C1 H1A 0.9900 .
C1 H1B 0.9900 .
P1 C12 1.8507(12) .
P1 C31 1.8622(13) .
P1 C32 1.8698(12) .
C14 C15 1.3860(19) .
C14 C13 1.3863(18) .
C14 H14 0.9500 .
C31 C33 1.5278(18) .
C31 C34 1.5308(17) .
C31 H31 1.0000 .
C32 C35 1.5234(18) .
C32 C36 1.5300(18) .
C32 H32 1.0000 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C16 C15 1.3862(19) .
C16 C11 1.3971(17) .
C16 H16 0.9500 .
C15 H15 0.9500 .
C13 C12 1.4029(17) .
C13 H13 0.9500 .
C12 C11 1.4107(17) .
