#------------------------------------------------------------------------------
#$Date: 2017-05-06 00:39:41 +0300 (Sat, 06 May 2017) $
#$Revision: 196311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/41/1544198.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_1544198
loop_
_publ_author_name
'Adachi, Shinya'
'Kumagai, Naoya'
'Shibasaki, Masakatsu'
_publ_section_title
;
 Pyramidalization/twisting of the amide functional group via remote steric
 congestion triggered by metal coordination.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              85
_journal_page_last               90
_journal_paper_doi               10.1039/c6sc03669d
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C46 H42 N6 O2 Pd'
_chemical_formula_sum            'C46 H42 N6 O2 Pd'
_chemical_formula_weight         817.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_update_record
;
2016-07-20 deposited with the CCDC.
2016-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                101.284(7)
_cell_angle_beta                 100.453(7)
_cell_angle_gamma                102.182(7)
_cell_formula_units_Z            1
_cell_length_a                   8.88787(16)
_cell_length_b                   10.65997(19)
_cell_length_c                   12.1038(2)
_cell_measurement_reflns_used    10321
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      3.83
_cell_volume                     1069.19(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12558
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         3.829
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.832
_exptl_absorpt_correction_T_max  0.465
_exptl_absorpt_correction_T_min  0.336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             422.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0697P)²+0.0302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3289
_reflns_number_total             3851
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c6sc03669d2.cif
_cod_data_source_block           160330adachi3
_cod_depositor_comments
;Adding full bibliography for 1544197--1544204.cif.

 Adding full bibliography for 1544197--1544204.cif.
;
_cod_database_code               1544198
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.5000 1.0000 0.03777(18) Uani 1 2 d S . P
O3 O 0.2533(4) 0.5834(4) 0.7975(3) 0.0565(9) Uani 1 1 d . . .
N4 N 0.6772(4) 0.5587(3) 0.9229(3) 0.0355(8) Uani 1 1 d . . .
N5 N 0.4571(4) 0.4941(4) 0.7650(3) 0.0409(9) Uani 1 1 d . . .
N34 N 0.4003(4) 0.4048(3) 0.8351(3) 0.0375(9) Uani 1 1 d . . .
C9 C 0.8902(5) 0.5877(5) 0.7860(4) 0.0450(12) Uani 1 1 d . . .
H9 H 0.9655 0.5992 0.7398 0.054 Uiso 1 1 calc R U .
C10 C 0.3093(5) 0.2910(4) 0.7780(4) 0.0371(10) Uani 1 1 d . . .
C11 C 0.6719(6) 0.4930(5) 0.6034(4) 0.0484(12) Uani 1 1 d . . .
H11A H 0.7622 0.5068 0.5673 0.058 Uiso 1 1 calc R U .
H11B H 0.6186 0.3985 0.5836 0.058 Uiso 1 1 calc R U .
H11C H 0.5974 0.5419 0.5751 0.058 Uiso 1 1 calc R U .
C12 C 0.8339(5) 0.5970(4) 0.9696(4) 0.0399(11) Uani 1 1 d . . .
H12 H 0.8706 0.6111 1.0509 0.048 Uiso 1 1 calc R U .
C13 C 0.7285(5) 0.5413(5) 0.7314(4) 0.0419(11) Uani 1 1 d . . .
C14 C 0.2332(5) 0.2613(5) 0.6521(4) 0.0435(11) Uani 1 1 d . . .
C15 C 0.4324(6) 0.6953(5) 0.7053(5) 0.0484(12) Uani 1 1 d . . .
H15 H 0.5237 0.6943 0.6751 0.058 Uiso 1 1 calc R U .
C16 C 0.2730(5) 0.1884(5) 0.8411(4) 0.0441(11) Uani 1 1 d . . .
C17 C 0.6263(5) 0.5346(4) 0.8059(4) 0.0405(11) Uani 1 1 d . . .
C18 C 0.0259(6) 0.2821(6) 0.5029(5) 0.0591(15) Uani 1 1 d . . .
H18 H -0.0599 0.3188 0.4802 0.071 Uiso 1 1 calc R U .
C19 C 0.1068(6) 0.3145(6) 0.6178(4) 0.0547(14) Uani 1 1 d . . .
H19 H 0.0760 0.3734 0.6739 0.066 Uiso 1 1 calc R U .
C20 C 0.1208(6) 0.1026(5) 0.8104(5) 0.0492(12) Uani 1 1 d . . .
H20 H 0.0432 0.1088 0.7479 0.059 Uiso 1 1 calc R U .
C21 C 0.3725(5) 0.5929(5) 0.7604(4) 0.0458(12) Uani 1 1 d . . .
C22 C 0.3860(6) 0.1763(5) 0.9325(5) 0.0512(13) Uani 1 1 d . . .
H22 H 0.4899 0.2330 0.9535 0.061 Uiso 1 1 calc R U .
C23 C 0.3444(7) 0.0799(5) 0.9927(5) 0.0535(13) Uani 1 1 d . . .
H23 H 0.4201 0.0721 1.0557 0.064 Uiso 1 1 calc R U .
C24 C 0.0700(6) 0.1965(5) 0.4217(5) 0.0563(14) Uani 1 1 d . . .
H24 H 0.0124 0.1724 0.3432 0.068 Uiso 1 1 calc R U .
C26 C 0.3598(6) 0.7899(6) 0.6971(5) 0.0608(15) Uani 1 1 d . . .
H26 H 0.2716 0.7888 0.7314 0.073 Uiso 1 1 calc R U .
C27 C 0.2795(6) 0.1792(5) 0.5691(4) 0.0541(13) Uani 1 1 d . . .
H27 H 0.3680 0.1451 0.5907 0.065 Uiso 1 1 calc R U .
C28 C 0.0856(7) 0.0086(5) 0.8726(5) 0.0612(15) Uani 1 1 d . . .
H28 H -0.0176 -0.0492 0.8530 0.073 Uiso 1 1 calc R U .
C29 C 0.1976(7) -0.0023(5) 0.9621(5) 0.0593(14) Uani 1 1 d . . .
H29 H 0.1715 -0.0683 1.0030 0.071 Uiso 1 1 calc R U .
C30 C 0.1962(7) 0.1458(5) 0.4528(5) 0.0580(14) Uani 1 1 d . . .
H30 H 0.2272 0.0882 0.3960 0.070 Uiso 1 1 calc R U .
C31 C 0.4035(7) 0.8979(6) 0.6393(7) 0.085(2) Uani 1 1 d . . .
H31A H 0.3307 0.9550 0.6456 0.102 Uiso 1 1 calc R U .
H31B H 0.5119 0.9502 0.6767 0.102 Uiso 1 1 calc R U .
H31C H 0.3967 0.8601 0.5575 0.102 Uiso 1 1 calc R U .
C35 C 0.9420(5) 0.6163(5) 0.9031(4) 0.0422(11) Uani 1 1 d . . .
H35 H 1.0518 0.6493 0.9383 0.051 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Pd Pd 0.1215 3.9337
;
International Tables for Crystallography
(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
N34 Pd1 N34 180.0(2) . 2_667
N34 Pd1 N4 100.95(14) . 2_667
N34 Pd1 N4 79.05(14) 2_667 2_667
N34 Pd1 N4 79.05(14) . .
N34 Pd1 N4 100.95(15) 2_667 .
N4 Pd1 N4 180.0 2_667 .
C12 N4 C17 118.5(4) . .
C12 N4 Pd1 128.2(3) . .
C17 N4 Pd1 112.4(3) . .
C21 N5 C17 118.8(4) . .
C21 N5 N34 112.1(3) . .
C17 N5 N34 105.6(3) . .
C10 N34 N5 115.7(4) . .
C10 N34 Pd1 138.1(3) . .
N5 N34 Pd1 106.2(2) . .
C35 C9 C13 121.9(4) . .
C35 C9 H9 119.1 . .
C13 C9 H9 119.1 . .
N34 C10 C16 118.3(4) . .
N34 C10 C14 122.9(4) . .
C16 C10 C14 118.7(4) . .
C13 C11 H11A 109.5 . .
C13 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C13 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N4 C12 C35 121.8(4) . .
N4 C12 H12 119.1 . .
C35 C12 H12 119.1 . .
C17 C13 C9 115.1(4) . .
C17 C13 C11 122.5(4) . .
C9 C13 C11 122.2(4) . .
C27 C14 C19 119.0(5) . .
C27 C14 C10 122.3(4) . .
C19 C14 C10 118.7(4) . .
C26 C15 C21 119.7(5) . .
C26 C15 H15 120.1 . .
C21 C15 H15 120.1 . .
C22 C16 C20 119.5(5) . .
C22 C16 C10 121.3(4) . .
C20 C16 C10 119.1(4) . .
N4 C17 C13 123.2(4) . .
N4 C17 N5 114.1(4) . .
C13 C17 N5 122.6(4) . .
C24 C18 C19 119.8(5) . .
C24 C18 H18 120.1 . .
C19 C18 H18 120.1 . .
C18 C19 C14 120.6(5) . .
C18 C19 H19 119.7 . .
C14 C19 H19 119.7 . .
C28 C20 C16 118.9(5) . .
C28 C20 H20 120.5 . .
C16 C20 H20 120.5 . .
O3 C21 N5 119.1(5) . .
O3 C21 C15 124.6(4) . .
N5 C21 C15 116.2(4) . .
C23 C22 C16 119.3(5) . .
C23 C22 H22 120.3 . .
C16 C22 H22 120.3 . .
C29 C23 C22 120.6(5) . .
C29 C23 H23 119.7 . .
C22 C23 H23 119.7 . .
C30 C24 C18 120.6(5) . .
C30 C24 H24 119.7 . .
C18 C24 H24 119.7 . .
C15 C26 C31 125.8(6) . .
C15 C26 H26 117.1 . .
C31 C26 H26 117.1 . .
C14 C27 C30 120.2(5) . .
C14 C27 H27 119.9 . .
C30 C27 H27 119.9 . .
C29 C28 C20 121.0(5) . .
C29 C28 H28 119.5 . .
C20 C28 H28 119.5 . .
C23 C29 C28 120.7(5) . .
C23 C29 H29 119.7 . .
C28 C29 H29 119.7 . .
C24 C30 C27 119.8(5) . .
C24 C30 H30 120.1 . .
C27 C30 H30 120.1 . .
C26 C31 H31A 109.5 . .
C26 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C26 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C9 C35 C12 119.1(4) . .
C9 C35 H35 120.4 . .
C12 C35 H35 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N34 1.996(4) .
Pd1 N34 1.996(4) 2_667
Pd1 N4 2.022(4) 2_667
Pd1 N4 2.023(4) .
O3 C21 1.216(5) .
N4 C12 1.346(5) .
N4 C17 1.360(6) .
N5 C21 1.421(6) .
N5 C17 1.438(5) .
N5 N34 1.466(5) .
N34 C10 1.288(5) .
C9 C35 1.359(7) .
C9 C13 1.405(6) .
C9 H9 0.9500 .
C10 C16 1.466(6) .
C10 C14 1.492(6) .
C11 C13 1.487(6) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C35 1.369(6) .
C12 H12 0.9500 .
C13 C17 1.392(6) .
C14 C27 1.379(7) .
C14 C19 1.395(7) .
C15 C26 1.317(7) .
C15 C21 1.444(7) .
C15 H15 0.9500 .
C16 C22 1.399(7) .
C16 C20 1.403(7) .
C18 C24 1.376(7) .
C18 C19 1.384(7) .
C18 H18 0.9500 .
C19 H19 0.9500 .
C20 C28 1.385(7) .
C20 H20 0.9500 .
C22 C23 1.398(7) .
C22 H22 0.9500 .
C23 C29 1.350(7) .
C23 H23 0.9500 .
C24 C30 1.369(7) .
C24 H24 0.9500 .
C26 C31 1.480(8) .
C26 H26 0.9500 .
C27 C30 1.404(7) .
C27 H27 0.9500 .
C28 C29 1.373(8) .
C28 H28 0.9500 .
C29 H29 0.9500 .
C30 H30 0.9500 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C35 H35 0.9500 .
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
C21 N5 N34 C10 102.0(4)
C17 N5 N34 C10 -127.2(4)
C21 N5 N34 Pd1 -80.1(3)
C17 N5 N34 Pd1 50.7(3)
N5 N34 C10 C16 168.6(3)
Pd1 N34 C10 C16 -8.4(6)
N5 N34 C10 C14 -14.5(5)
Pd1 N34 C10 C14 168.5(3)
C17 N4 C12 C35 2.1(6)
Pd1 N4 C12 C35 170.5(3)
C35 C9 C13 C17 3.5(7)
C35 C9 C13 C11 -171.8(5)
N34 C10 C14 C27 109.1(6)
C16 C10 C14 C27 -74.0(6)
N34 C10 C14 C19 -73.5(6)
C16 C10 C14 C19 103.4(5)
N34 C10 C16 C22 -36.0(6)
C14 C10 C16 C22 147.0(4)
N34 C10 C16 C20 142.7(4)
C14 C10 C16 C20 -34.3(6)
C12 N4 C17 C13 3.3(6)
Pd1 N4 C17 C13 -166.9(4)
C12 N4 C17 N5 179.9(4)
Pd1 N4 C17 N5 9.8(4)
C9 C13 C17 N4 -6.0(7)
C11 C13 C17 N4 169.3(4)
C9 C13 C17 N5 177.7(4)
C11 C13 C17 N5 -7.0(7)
C21 N5 C17 N4 87.0(5)
N34 N5 C17 N4 -39.8(5)
C21 N5 C17 C13 -96.3(5)
N34 N5 C17 C13 136.8(4)
C24 C18 C19 C14 0.1(9)
C27 C14 C19 C18 2.0(8)
C10 C14 C19 C18 -175.5(5)
C22 C16 C20 C28 0.7(7)
C10 C16 C20 C28 -178.0(4)
C17 N5 C21 O3 -134.1(5)
N34 N5 C21 O3 -10.4(6)
C17 N5 C21 C15 49.0(6)
N34 N5 C21 C15 172.7(4)
C26 C15 C21 O3 2.9(8)
C26 C15 C21 N5 179.6(5)
C20 C16 C22 C23 -0.8(7)
C10 C16 C22 C23 177.8(4)
C16 C22 C23 C29 1.0(7)
C19 C18 C24 C30 -1.8(9)
C21 C15 C26 C31 -177.5(5)
C19 C14 C27 C30 -2.5(8)
C10 C14 C27 C30 174.9(5)
C16 C20 C28 C29 -0.8(8)
C22 C23 C29 C28 -1.0(8)
C20 C28 C29 C23 0.9(8)
C18 C24 C30 C27 1.3(9)
C14 C27 C30 C24 0.9(8)
C13 C9 C35 C12 1.4(7)
N4 C12 C35 C9 -4.4(7)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.251 0.786 0.233 55 41 ' '
2 0.749 0.214 0.767 55 41 ' '
