#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/08/7000802.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_7000802
loop_
_publ_author_name
'Han, Yuan'
'Huynh, Han Vinh'
_publ_section_title
;
 Mixed carbene--isocyanide Pd(ii) complexes: synthesis, structures and
 reactivity towards nucleophiles
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2201
_journal_page_last               2209
_journal_paper_doi               10.1039/b816471a
_journal_year                    2009
_chemical_formula_sum            'C25 H29 N3'
_chemical_formula_weight         371.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.6700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.2291(15)
_cell_length_b                   13.0532(9)
_cell_length_c                   17.1124(12)
_cell_measurement_reflns_used    1188
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      20.51
_cell_measurement_theta_min      2.44
_cell_volume                     4367.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12607
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9934
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.127
_refine_diff_density_min         -0.095
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+1.4394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                2169
_reflns_number_total             3844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816471a.txt
_cod_data_source_block           6303
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7000802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.23447(10) 1.02759(18) 0.17449(15) 0.0614(6) Uani 1 1 d . . .
N2 N 0.12925(11) 0.96361(19) 0.06368(17) 0.0600(7) Uani 1 1 d . . .
H2A H 0.1086(11) 0.9226(18) 0.0243(15) 0.043(8) Uiso 1 1 d . . .
N3 N 0.22447(12) 0.88930(17) 0.08021(15) 0.0554(6) Uani 1 1 d . . .
H3A H 0.2665(14) 0.888(2) 0.1059(18) 0.077(10) Uiso 1 1 d . . .
C1 C 0.19905(11) 0.9631(2) 0.11013(17) 0.0476(6) Uani 1 1 d . . .
C2 C 0.30694(12) 1.0262(2) 0.22101(18) 0.0605(7) Uani 1 1 d . . .
C3 C 0.33889(14) 1.0952(2) 0.1938(2) 0.0713(8) Uani 1 1 d . . .
C4 C 0.40971(16) 1.1018(3) 0.2451(3) 0.0898(10) Uani 1 1 d . . .
H4 H 0.4312 1.1485 0.2270 0.108 Uiso 1 1 calc R . .
C5 C 0.44870(16) 1.0415(3) 0.3213(3) 0.0929(11) Uani 1 1 d . . .
H5 H 0.4966 1.0464 0.3552 0.112 Uiso 1 1 calc R . .
C6 C 0.41729(15) 0.9736(3) 0.3481(2) 0.0869(10) Uani 1 1 d . . .
H6 H 0.4442 0.9324 0.4007 0.104 Uiso 1 1 calc R . .
C7 C 0.34634(14) 0.9650(2) 0.2988(2) 0.0678(8) Uani 1 1 d . . .
C8 C 0.29703(16) 1.1651(3) 0.1119(2) 0.1046(12) Uani 1 1 d . . .
H8A H 0.3272 1.2108 0.1056 0.157 Uiso 1 1 calc R . .
H8B H 0.2661 1.2049 0.1213 0.157 Uiso 1 1 calc R . .
H8C H 0.2709 1.1243 0.0559 0.157 Uiso 1 1 calc R . .
C9 C 0.31329(16) 0.8921(3) 0.3308(2) 0.0935(10) Uani 1 1 d . . .
H9A H 0.2751 0.9258 0.3284 0.140 Uiso 1 1 calc R . .
H9B H 0.3465 0.8711 0.3941 0.140 Uiso 1 1 calc R . .
H9C H 0.2970 0.8324 0.2908 0.140 Uiso 1 1 calc R . .
C10 C 0.09097(11) 1.0328(2) 0.08312(18) 0.0593(7) Uani 1 1 d . . .
C11 C 0.07027(13) 1.0010(3) 0.1416(2) 0.0724(9) Uani 1 1 d . . .
C12 C 0.02949(16) 1.0665(4) 0.1552(2) 0.0962(13) Uani 1 1 d . . .
H12 H 0.0152 1.0467 0.1950 0.115 Uiso 1 1 calc R . .
C13 C 0.00978(16) 1.1595(4) 0.1119(3) 0.1067(16) Uani 1 1 d . . .
H13 H -0.0183 1.2026 0.1215 0.128 Uiso 1 1 calc R . .
C14 C 0.03073(15) 1.1901(3) 0.0545(3) 0.0946(12) Uani 1 1 d . . .
H14 H 0.0173 1.2546 0.0256 0.113 Uiso 1 1 calc R . .
C15 C 0.07146(13) 1.1272(2) 0.0385(2) 0.0719(9) Uani 1 1 d . . .
C16 C 0.09142(17) 0.8991(3) 0.1892(2) 0.0973(11) Uani 1 1 d . . .
H16A H 0.0747 0.8922 0.2301 0.146 Uiso 1 1 calc R . .
H16B H 0.1409 0.8941 0.2253 0.146 Uiso 1 1 calc R . .
H16C H 0.0723 0.8449 0.1432 0.146 Uiso 1 1 calc R . .
C17 C 0.09331(16) 1.1603(3) -0.0256(3) 0.1015(11) Uani 1 1 d . . .
H17A H 0.0704 1.2237 -0.0560 0.152 Uiso 1 1 calc R . .
H17B H 0.0813 1.1077 -0.0721 0.152 Uiso 1 1 calc R . .
H17C H 0.1424 1.1708 0.0097 0.152 Uiso 1 1 calc R . .
C18 C 0.18549(12) 0.8171(2) 0.00692(18) 0.0531(7) Uani 1 1 d . . .
C19 C 0.16530(14) 0.7257(2) 0.0258(2) 0.0660(8) Uani 1 1 d . . .
C20 C 0.12966(16) 0.6562(3) -0.0459(3) 0.0903(10) Uani 1 1 d . . .
H20 H 0.1153 0.5940 -0.0341 0.108 Uiso 1 1 calc R . .
C21 C 0.11489(15) 0.6756(3) -0.1327(3) 0.0954(12) Uani 1 1 d . . .
H21 H 0.0909 0.6269 -0.1799 0.114 Uiso 1 1 calc R . .
C22 C 0.13490(16) 0.7664(3) -0.1518(2) 0.0857(11) Uani 1 1 d . . .
H22 H 0.1247 0.7793 -0.2120 0.103 Uiso 1 1 calc R . .
C23 C 0.17039(13) 0.8396(3) -0.0818(2) 0.0660(8) Uani 1 1 d . . .
C24 C 0.18175(19) 0.7007(3) 0.1215(2) 0.1017(11) Uani 1 1 d . . .
H24A H 0.2306 0.6894 0.1627 0.152 Uiso 1 1 calc R . .
H24B H 0.1573 0.6392 0.1191 0.152 Uiso 1 1 calc R . .
H24C H 0.1680 0.7572 0.1447 0.152 Uiso 1 1 calc R . .
C25 C 0.19109(18) 0.9400(3) -0.1021(2) 0.0968(11) Uani 1 1 d . . .
H25A H 0.1644 0.9948 -0.0983 0.145 Uiso 1 1 calc R . .
H25B H 0.1829 0.9383 -0.1640 0.145 Uiso 1 1 calc R . .
H25C H 0.2393 0.9520 -0.0570 0.145 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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C1 N1 C2 119.5(2) . . ?
C1 N2 C10 124.1(2) . . ?
C1 N3 C18 126.5(2) . . ?
N1 C1 N3 125.6(2) . . ?
N1 C1 N2 120.6(2) . . ?
N3 C1 N2 113.8(2) . . ?
C7 C2 C3 119.7(3) . . ?
C7 C2 N1 120.8(3) . . ?
C3 C2 N1 119.1(3) . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 C8 120.0(3) . . ?
C2 C3 C8 120.5(3) . . ?
C5 C4 C3 121.1(3) . . ?
C4 C5 C6 119.5(3) . . ?
C5 C6 C7 121.1(3) . . ?
C2 C7 C6 119.1(3) . . ?
C2 C7 C9 120.8(3) . . ?
C6 C7 C9 120.1(3) . . ?
C11 C10 C15 121.6(3) . . ?
C11 C10 N2 118.8(3) . . ?
C15 C10 N2 119.5(3) . . ?
C12 C11 C10 118.1(4) . . ?
C12 C11 C16 120.6(3) . . ?
C10 C11 C16 121.3(3) . . ?
C13 C12 C11 121.0(4) . . ?
C12 C13 C14 120.2(3) . . ?
C13 C14 C15 120.9(4) . . ?
C14 C15 C10 118.1(3) . . ?
C14 C15 C17 120.7(3) . . ?
C10 C15 C17 121.3(3) . . ?
C19 C18 C23 121.3(3) . . ?
C19 C18 N3 119.8(2) . . ?
C23 C18 N3 118.9(3) . . ?
C18 C19 C20 118.3(3) . . ?
C18 C19 C24 121.6(3) . . ?
C20 C19 C24 120.1(3) . . ?
C21 C20 C19 121.7(4) . . ?
C20 C21 C22 120.3(4) . . ?
C21 C22 C23 120.2(3) . . ?
C18 C23 C22 118.3(3) . . ?
C18 C23 C25 120.8(3) . . ?
C22 C23 C25 120.9(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.273(3) . ?
N1 C2 1.422(3) . ?
N2 C1 1.367(3) . ?
N2 C10 1.427(3) . ?
N3 C1 1.365(3) . ?
N3 C18 1.433(3) . ?
C2 C7 1.390(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.387(4) . ?
C3 C8 1.507(4) . ?
C4 C5 1.366(5) . ?
C5 C6 1.375(4) . ?
C6 C7 1.393(4) . ?
C7 C9 1.500(4) . ?
C10 C11 1.387(4) . ?
C10 C15 1.390(4) . ?
C11 C12 1.387(4) . ?
C11 C16 1.498(4) . ?
C12 C13 1.366(5) . ?
C13 C14 1.371(5) . ?
C14 C15 1.387(4) . ?
C15 C17 1.499(4) . ?
C18 C19 1.382(4) . ?
C18 C23 1.393(3) . ?
C19 C20 1.385(4) . ?
C19 C24 1.504(4) . ?
C20 C21 1.355(4) . ?
C21 C22 1.375(5) . ?
C22 C23 1.400(4) . ?
C23 C25 1.500(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 25945298
