#------------------------------------------------------------------------------
#$Date: 2016-08-07 10:45:47 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185091 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543272.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_1543272
loop_
_publ_author_name
'Singh, Karandeep'
'Singh, Ajay K.'
'Singh, Devendra'
'Singh, Rakhi'
'Sharma, Siddharth'
_publ_section_title
;
 Pd/Fe3O4supported on nitrogen-doped reduced graphene oxide for
 room-temperature isocyanide insertion reactions
;
_journal_issue                   11
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              3723
_journal_paper_doi               10.1039/C5CY01973G
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C23 H15 N'
_chemical_formula_weight         305.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-17 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.533(4)
_cell_length_b                   7.5052(15)
_cell_length_c                   21.247(4)
_cell_measurement_temperature    296(2)
_cell_volume                     3114.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46038
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.136
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0910P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                1741
_reflns_number_total             3545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cy01973g2.cif
_cod_data_source_block           l13_07
_cod_depositor_comments          'Adding full bibliography for 1543272.cif.'
_cod_original_cell_volume        3114.9(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1543272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
N1 N 0.17061(9) 0.6715(2) 0.13160(8) 0.0605(5) Uani 1 1 d .
C18 C 0.12517(11) 0.8212(3) -0.09931(9) 0.0549(5) Uani 1 1 d .
C6 C 0.24397(10) 0.7225(3) 0.03908(9) 0.0518(5) Uani 1 1 d .
C23 C 0.18405(10) 0.7526(3) -0.06787(9) 0.0508(5) Uani 1 1 d .
C9 C 0.11633(11) 0.7111(3) 0.09752(9) 0.0551(5) Uani 1 1 d .
C22 C 0.23719(11) 0.6876(3) -0.10599(10) 0.0595(6) Uani 1 1 d .
H22 H 0.2747 0.6329 -0.0872 0.071 Uiso 1 1 calc R
C17 C 0.06534(11) 0.8603(3) -0.06395(10) 0.0603(6) Uani 1 1 d .
H17 H 0.0283 0.9144 -0.0837 0.072 Uiso 1 1 calc R
C8 C 0.11988(10) 0.7556(3) 0.03156(9) 0.0514(5) Uani 1 1 d .
C16 C 0.06153(11) 0.8197(3) -0.00165(10) 0.0573(6) Uani 1 1 d .
H16 H 0.0202 0.8340 0.0195 0.069 Uiso 1 1 calc R
C10 C 0.04951(11) 0.7078(3) 0.13187(9) 0.0564(5) Uani 1 1 d .
C19 C 0.12544(12) 0.8392(3) -0.16504(10) 0.0622(6) Uani 1 1 d .
H19 H 0.0877 0.8897 -0.1850 0.075 Uiso 1 1 calc R
C7 C 0.18305(10) 0.7417(3) 0.00032(10) 0.0513(5) Uani 1 1 d .
C5 C 0.31152(11) 0.7574(3) 0.01836(11) 0.0595(6) Uani 1 1 d .
H5 H 0.3189 0.7919 -0.0231 0.071 Uiso 1 1 calc R
C1 C 0.23393(11) 0.6840(3) 0.10350(10) 0.0581(6) Uani 1 1 d .
C13 C -0.07221(13) 0.7015(3) 0.20087(11) 0.0711(7) Uani 1 1 d .
H13 H -0.1127 0.6996 0.2239 0.085 Uiso 1 1 calc R
C20 C 0.17978(13) 0.7844(3) -0.20027(11) 0.0704(7) Uani 1 1 d .
H20 H 0.1800 0.8012 -0.2436 0.084 Uiso 1 1 calc R
C11 C 0.04369(12) 0.7963(3) 0.18934(9) 0.0599(6) Uani 1 1 d .
H11 H 0.0810 0.8588 0.2052 0.072 Uiso 1 1 calc R
C21 C 0.23492(12) 0.7029(3) -0.17037(10) 0.0675(6) Uani 1 1 d .
H21 H 0.2708 0.6582 -0.1944 0.081 Uiso 1 1 calc R
C2 C 0.29148(12) 0.6611(3) 0.14254(11) 0.0714(7) Uani 1 1 d .
H2 H 0.2852 0.6272 0.1842 0.086 Uiso 1 1 calc R
C12 C -0.01654(12) 0.7924(3) 0.22301(10) 0.0657(6) Uani 1 1 d .
H12 H -0.0194 0.8523 0.2612 0.079 Uiso 1 1 calc R
C15 C -0.00733(12) 0.6153(3) 0.11002(10) 0.0665(6) Uani 1 1 d .
H15 H -0.0047 0.5544 0.0720 0.080 Uiso 1 1 calc R
C14 C -0.06782(12) 0.6122(3) 0.14392(12) 0.0721(7) Uani 1 1 d .
H14 H -0.1055 0.5502 0.1285 0.086 Uiso 1 1 calc R
C4 C 0.36607(12) 0.7413(3) 0.05833(11) 0.0699(6) Uani 1 1 d .
H4 H 0.4100 0.7661 0.0440 0.084 Uiso 1 1 calc R
C3 C 0.35605(12) 0.6876(4) 0.12068(12) 0.0759(7) Uani 1 1 d .
H3 H 0.3934 0.6701 0.1471 0.091 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
C9 N1 C1 117.97(17)
C19 C18 C17 120.64(19)
C19 C18 C23 119.9(2)
C17 C18 C23 119.37(19)
C1 C6 C5 117.96(18)
C1 C6 C7 117.08(18)
C5 C6 C7 124.62(19)
C22 C23 C18 116.83(18)
C22 C23 C7 124.47(19)
C18 C23 C7 118.51(19)
N1 C9 C8 123.20(19)
N1 C9 C10 115.48(18)
C8 C9 C10 121.32(18)
C21 C22 C23 121.4(2)
C16 C17 C18 120.90(19)
C7 C8 C16 119.59(18)
C7 C8 C9 118.94(18)
C16 C8 C9 121.42(19)
C17 C16 C8 120.9(2)
C15 C10 C11 117.7(2)
C15 C10 C9 122.86(18)
C11 C10 C9 119.39(19)
C20 C19 C18 121.4(2)
C8 C7 C23 118.64(18)
C8 C7 C6 117.29(17)
C23 C7 C6 124.05(18)
C4 C5 C6 121.1(2)
N1 C1 C2 116.97(19)
N1 C1 C6 123.99(18)
C2 C1 C6 119.0(2)
C12 C13 C14 119.5(2)
C19 C20 C21 119.0(2)
C12 C11 C10 121.0(2)
C22 C21 C20 121.1(2)
C3 C2 C1 121.5(2)
C13 C12 C11 120.7(2)
C14 C15 C10 121.1(2)
C15 C14 C13 119.9(2)
C5 C4 C3 120.3(2)
C2 C3 C4 119.7(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C9 1.318(3)
N1 C1 1.377(3)
C18 C19 1.403(3)
C18 C17 1.420(3)
C18 C23 1.426(3)
C6 C1 1.412(3)
C6 C5 1.415(3)
C6 C7 1.454(3)
C23 C22 1.404(3)
C23 C7 1.451(3)
C9 C8 1.442(3)
C9 C10 1.496(3)
C22 C21 1.374(3)
C17 C16 1.360(3)
C8 C7 1.405(3)
C8 C16 1.424(3)
C10 C15 1.390(3)
C10 C11 1.394(3)
C19 C20 1.362(3)
C5 C4 1.368(3)
C1 C2 1.408(3)
C13 C12 1.367(3)
C13 C14 1.386(3)
C20 C21 1.392(3)
C11 C12 1.377(3)
C2 C3 1.359(3)
C15 C14 1.384(3)
C4 C3 1.398(3)
