#------------------------------------------------------------------------------
#$Date: 2018-10-29 09:33:49 +0200 (Mon, 29 Oct 2018) $
#$Revision: 211691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/28/7032889.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_7032889
loop_
_publ_author_name
'Maity, Ramananda'
'van der Meer, Margarethe'
'Sarkar, Biprajit'
_publ_section_title
;
 Redox-active multinuclear Pd(II) complexes with bis- and tris-mesoionic
 carbenes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              46
_journal_page_last               49
_journal_paper_doi               10.1039/c4dt03239j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C28 H22 Cl6 I5 N8 Pd2'
_chemical_formula_weight         1403.64
_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                 91.044(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.427(5)
_cell_length_b                   11.379(4)
_cell_length_c                   24.293(8)
_cell_measurement_reflns_used    3199
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      1.68
_cell_volume                     4264(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       '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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17194
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    4.146
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.222
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0521
_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)+(0.0275P)²+134.9888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                3199
_reflns_number_total             3796
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt03239j2.cif
_cod_data_source_block           sar499
_cod_depositor_comments
;
Adding full bibliography for 7032889--7032891.cif.

2018-09-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C18.67 H14.67 Cl4 I2.67 N5.33 Pd1.33'
_cod_original_formula_weight         935.76
_cod_original_formula_units_Z            6
_cod_original_cell_volume        4264(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7032889
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
I1 I 0.29912(4) -0.01777(6) 0.02390(3) 0.0316(2) Uani 1 1 d .
I2 I 0.13857(4) 0.04074(6) 0.20920(3) 0.02885(19) Uani 1 1 d .
Pd1 Pd 0.22732(4) 0.01590(6) 0.11876(3) 0.02034(19) Uani 1 1 d .
Cl2 Cl 0.5919(2) -0.1476(3) 0.09554(14) 0.0503(8) Uani 1 1 d .
Cl1 Cl 0.4823(2) -0.0566(5) 0.17873(16) 0.0754(13) Uani 1 1 d .
Cl3 Cl 0.66668(18) -0.0848(2) 0.20204(12) 0.0392(6) Uani 1 1 d .
C5 C 0.0451(6) -0.0787(8) 0.0344(4) 0.0197(19) Uani 1 1 d .
C7 C -0.0253(6) -0.0350(8) -0.0531(4) 0.0218(19) Uani 1 1 d .
H7 H -0.0420 -0.0584 -0.0884 0.026 Uiso 1 1 calc R
N2 N 0.1306(5) -0.3250(7) 0.1138(4) 0.0260(18) Uani 1 1 d .
N3 N 0.0760(5) -0.2744(7) 0.0784(3) 0.0244(18) Uani 1 1 d .
N1 N 0.1825(5) -0.2373(7) 0.1299(3) 0.0222(17) Uani 1 1 d .
C50 C 0.5754(7) -0.1419(10) 0.1658(5) 0.043(3) Uani 1 1 d .
H50 H 0.5649 -0.2220 0.1790 0.052 Uiso 1 1 calc R
N4 N 0.2978(5) 0.1722(7) 0.1334(3) 0.0229(17) Uani 1 1 d .
C6 C 0.0196(6) -0.1131(8) -0.0182(4) 0.023(2) Uani 1 1 d .
H6 H 0.0324 -0.1884 -0.0305 0.028 Uiso 1 1 calc R
C10 C 0.3483(7) 0.3609(9) 0.1039(5) 0.034(3) Uani 1 1 d .
H10 H 0.3467 0.4213 0.0782 0.041 Uiso 1 1 calc R
C2 C 0.0942(7) -0.1574(8) 0.0718(4) 0.024(2) Uani 1 1 d .
C9 C 0.3003(7) 0.2597(8) 0.0960(5) 0.029(2) Uani 1 1 d .
H9 H 0.2681 0.2516 0.0635 0.034 Uiso 1 1 calc R
C1 C 0.1638(6) -0.1315(8) 0.1053(4) 0.023(2) Uani 1 1 d .
C12 C 0.3978(7) 0.2818(10) 0.1897(5) 0.036(3) Uani 1 1 d .
H12 H 0.4308 0.2868 0.2220 0.043 Uiso 1 1 calc R
C8 C 0.0072(6) -0.3480(8) 0.0539(4) 0.026(2) Uani 1 1 d .
H8A H 0.0285 -0.3858 0.0215 0.039 Uiso 1 1 calc R
H8B H -0.0418 -0.2998 0.0442 0.039 Uiso 1 1 calc R
H8C H -0.0099 -0.4065 0.0800 0.039 Uiso 1 1 calc R
C3 C 0.2550(7) -0.2670(9) 0.1677(5) 0.032(2) Uani 1 1 d .
C13 C 0.3448(7) 0.1834(9) 0.1788(5) 0.031(2) Uani 1 1 d .
H13 H 0.3430 0.1236 0.2048 0.037 Uiso 1 1 calc R
C4 C 0.3353(8) -0.3043(12) 0.1347(6) 0.048(3) Uani 1 1 d .
C11 C 0.3991(7) 0.3696(10) 0.1514(5) 0.038(3) Uani 1 1 d .
H11 H 0.4340 0.4352 0.1571 0.046 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'
Cl Cl 0.1484 0.1585 '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'
I I -0.4742 1.8119 '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
C1 Pd1 N4 178.8(3) . .
C1 Pd1 I1 86.9(3) . .
N4 Pd1 I1 92.7(2) . .
C1 Pd1 I2 88.0(3) . .
N4 Pd1 I2 92.5(2) . .
I1 Pd1 I2 173.48(3) . .
C6 C5 C7 119.8(8) . 5
C6 C5 C2 122.0(8) . .
C7 C5 C2 118.2(8) 5 .
C6 C7 C5 119.7(9) . 5
N3 N2 N1 103.7(7) . .
N2 N3 C2 111.7(8) . .
N2 N3 C8 117.4(8) . .
C2 N3 C8 130.9(8) . .
N2 N1 C1 114.1(8) . .
N2 N1 C3 117.1(8) . .
C1 N1 C3 128.6(8) . .
Cl2 C50 Cl1 109.3(6) . .
Cl2 C50 Cl3 111.9(7) . .
Cl1 C50 Cl3 110.6(7) . .
C13 N4 C9 118.1(9) . .
C13 N4 Pd1 119.8(7) . .
C9 N4 Pd1 122.0(7) . .
C5 C6 C7 120.5(9) . .
C9 C10 C11 118.0(11) . .
C1 C2 N3 107.4(8) . .
C1 C2 C5 128.6(8) . .
N3 C2 C5 123.9(8) . .
N4 C9 C10 122.9(10) . .
C2 C1 N1 103.2(8) . .
C2 C1 Pd1 131.8(7) . .
N1 C1 Pd1 125.1(7) . .
C11 C12 C13 117.9(10) . .
N1 C3 C4 110.3(9) . .
N4 C13 C12 123.0(10) . .
C12 C11 C10 120.0(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Pd1 2.6032(12) .
I2 Pd1 2.6250(12) .
Pd1 C1 1.967(10) .
Pd1 N4 2.111(8) .
Cl2 C50 1.732(14) .
Cl1 C50 1.766(12) .
Cl3 C50 1.771(12) .
C5 C6 1.389(13) .
C5 C7 1.407(13) 5
C5 C2 1.474(13) .
C7 C6 1.402(13) .
C7 C5 1.407(13) 5
N2 N3 1.325(11) .
N2 N1 1.334(11) .
N3 C2 1.371(12) .
N3 C8 1.469(12) .
N1 C1 1.373(12) .
N1 C3 1.472(12) .
N4 C13 1.315(13) .
N4 C9 1.349(13) .
C10 C9 1.381(14) .
C10 C11 1.385(17) .
C2 C1 1.367(14) .
C12 C11 1.367(17) .
C12 C13 1.409(14) .
C3 C4 1.546(16) .
