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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/70/1517036.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_1517036
loop_
_publ_author_name
'Shantanu Hazra'
'Biswarup Sarkar'
'Subrata Naiya'
'Michael G.B. Drew'
'Ashutosh Ghosh'
_publ_section_title
;
 Structural variations in the complexes of cadmium(II),
 hexamethylenetetramine, and 2-, 3- and 4-nitrobenzoates
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              12
_journal_page_last               19
_journal_volume                  402
_journal_year                    2013
_chemical_formula_sum            'C40 H46 Cd N12 O18'
_chemical_formula_weight         1095.29
_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
_cell_angle_alpha                84.717(14)
_cell_angle_beta                 75.307(15)
_cell_angle_gamma                85.07(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8716(19)
_cell_length_b                   11.583(3)
_cell_length_c                   12.6457(15)
_cell_measurement_reflns_used    7923
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.68
_cell_volume                     1108.2(4)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.1033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7923
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.335
_refine_diff_density_min         -2.540
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6210
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.1317P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                5545
_reflns_number_total             6210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-12-19-2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517036
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
C52 C -0.3535(4) -0.1228(3) 0.0180(3) 0.0185(6) Uani 1 1 d .
H52A H -0.3877 -0.0939 0.0905 0.022 Uiso 1 1 calc R
H52B H -0.3708 -0.0592 -0.0344 0.022 Uiso 1 1 calc R
C54 C -0.4103(4) -0.2584(3) -0.0980(3) 0.0206(7) Uani 1 1 d .
H54A H -0.4833 -0.3202 -0.1026 0.025 Uiso 1 1 calc R
H54B H -0.4281 -0.1955 -0.1511 0.025 Uiso 1 1 calc R
C56 C -0.2008(5) -0.3969(3) -0.0452(3) 0.0210(7) Uani 1 1 d .
H56A H -0.0786 -0.4264 -0.0631 0.025 Uiso 1 1 calc R
H56B H -0.2724 -0.4595 -0.0495 0.025 Uiso 1 1 calc R
C58 C -0.1400(4) -0.2630(3) 0.0727(3) 0.0168(6) Uani 1 1 d .
H58A H -0.0169 -0.2908 0.0568 0.020 Uiso 1 1 calc R
H58B H -0.1721 -0.2367 0.1462 0.020 Uiso 1 1 calc R
C59 C -0.1170(4) -0.2081(3) -0.1177(3) 0.0182(6) Uani 1 1 d .
H59A H -0.1314 -0.1448 -0.1712 0.022 Uiso 1 1 calc R
H59B H 0.0057 -0.2364 -0.1354 0.022 Uiso 1 1 calc R
C60 C -0.4358(4) -0.3131(3) 0.0927(3) 0.0205(7) Uani 1 1 d .
H60A H -0.5105 -0.3749 0.0909 0.025 Uiso 1 1 calc R
H60B H -0.4686 -0.2864 0.1660 0.025 Uiso 1 1 calc R
C12 C -0.1479(4) -0.0042(3) 0.2560(3) 0.0162(6) Uani 1 1 d .
C14 C -0.2521(4) 0.0599(3) 0.3525(3) 0.0144(6) Uani 1 1 d .
C15 C -0.2370(4) 0.0224(3) 0.4575(3) 0.0180(6) Uani 1 1 d .
H15 H -0.1619 -0.0415 0.4688 0.022 Uiso 1 1 calc R
C16 C -0.3344(4) 0.0811(3) 0.5441(3) 0.0182(6) Uani 1 1 d .
C17 C -0.4466(4) 0.1794(3) 0.5311(3) 0.0223(7) Uani 1 1 d .
H17 H -0.5109 0.2181 0.5914 0.027 Uiso 1 1 calc R
C18 C -0.4588(5) 0.2170(3) 0.4266(3) 0.0248(7) Uani 1 1 d .
H18 H -0.5320 0.2820 0.4157 0.030 Uiso 1 1 calc R
C19 C -0.3622(4) 0.1582(3) 0.3373(3) 0.0197(6) Uani 1 1 d .
H19 H -0.3709 0.1844 0.2670 0.024 Uiso 1 1 calc R
C31 C -0.2456(4) -0.5281(3) 0.5124(3) 0.0179(6) Uani 1 1 d .
H31 H -0.3302 -0.4670 0.5297 0.022 Uiso 1 1 calc R
C32 C -0.1790(4) -0.5563(3) 0.4048(3) 0.0166(6) Uani 1 1 d .
C33 C -0.0530(4) -0.6492(3) 0.3809(3) 0.0191(6) Uani 1 1 d .
H33 H -0.0090 -0.6682 0.3087 0.023 Uiso 1 1 calc R
C34 C 0.0072(5) -0.7137(3) 0.4645(3) 0.0230(7) Uani 1 1 d .
H34 H 0.0910 -0.7753 0.4475 0.028 Uiso 1 1 calc R
C35 C -0.0568(5) -0.6869(3) 0.5725(3) 0.0217(7) Uani 1 1 d .
H35 H -0.0176 -0.7293 0.6288 0.026 Uiso 1 1 calc R
C36 C -0.1821(4) -0.5937(3) 0.5937(3) 0.0183(6) Uani 1 1 d .
C41 C -0.2421(4) -0.4821(3) 0.3168(3) 0.0193(6) Uani 1 1 d .
N44 N -0.2453(4) -0.5608(3) 0.7069(3) 0.0239(6) Uani 1 1 d .
N51 N -0.1638(3) -0.1637(2) -0.0069(2) 0.0139(5) Uani 1 1 d .
N53 N -0.4658(3) -0.2160(3) 0.0137(3) 0.0205(6) Uani 1 1 d .
N55 N -0.2258(4) -0.3015(3) -0.1252(2) 0.0201(6) Uani 1 1 d .
N57 N -0.2488(4) -0.3598(3) 0.0680(2) 0.0166(5) Uani 1 1 d .
N20 N -0.3223(4) 0.0393(3) 0.6560(3) 0.0249(7) Uani 1 1 d .
O11 O -0.1768(3) 0.0329(2) 0.16441(19) 0.0206(5) Uani 1 1 d .
O13 O -0.0423(4) -0.0872(3) 0.2736(2) 0.0293(6) Uani 1 1 d .
O31 O -0.2486(4) -0.0579(3) 0.6690(2) 0.0333(7) Uani 1 1 d .
O32 O -0.3879(4) 0.1010(3) 0.7306(2) 0.0418(8) Uani 1 1 d .
O42 O -0.1901(4) -0.5243(2) 0.2196(2) 0.0224(5) Uani 1 1 d .
H42 H -0.2309 -0.4820 0.1753 0.027 Uiso 1 1 calc R
O43 O -0.3280(4) -0.3897(3) 0.3339(2) 0.0310(6) Uani 1 1 d .
O45 O -0.3627(4) -0.4819(3) 0.7263(2) 0.0309(6) Uani 1 1 d .
O46 O -0.1769(4) -0.6116(3) 0.7768(2) 0.0333(7) Uani 1 1 d .
Cd1 Cd 0.0000 0.0000 0.0000 0.01471(12) Uani 1 2 d S
O1 O 0.1800(3) -0.1284(3) 0.0789(2) 0.0249(6) Uani 1 1 d D
H1 H 0.285(3) -0.163(4) 0.064(3) 0.030 Uiso 1 1 d D
H2 H 0.139(5) -0.134(4) 0.1497(16) 0.030 Uiso 1 1 d 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
N53 C52 N51 111.8(3) . .
N55 C54 N53 111.9(3) . .
N55 C56 N57 112.1(3) . .
N57 C58 N51 111.7(3) . .
N55 C59 N51 112.2(3) . .
N53 C60 N57 112.1(3) . .
O13 C12 O11 126.9(3) . .
O13 C12 C14 117.9(3) . .
O11 C12 C14 115.3(3) . .
C15 C14 C19 119.6(3) . .
C15 C14 C12 119.9(3) . .
C19 C14 C12 120.6(3) . .
C16 C15 C14 118.8(3) . .
C15 C16 C17 122.7(3) . .
C15 C16 N20 118.9(3) . .
C17 C16 N20 118.4(3) . .
C18 C17 C16 118.1(3) . .
C17 C18 C19 120.3(3) . .
C18 C19 C14 120.5(3) . .
C32 C31 C36 118.0(3) . .
C31 C32 C33 120.0(3) . .
C31 C32 C41 117.9(3) . .
C33 C32 C41 122.1(3) . .
C34 C33 C32 120.5(3) . .
C35 C34 C33 120.6(3) . .
C34 C35 C36 117.5(3) . .
C31 C36 C35 123.4(3) . .
C31 C36 N44 118.4(3) . .
C35 C36 N44 118.2(3) . .
O43 C41 O42 123.9(3) . .
O43 C41 C32 122.7(3) . .
O42 C41 C32 113.4(3) . .
O46 N44 O45 123.6(3) . .
O46 N44 C36 118.3(3) . .
O45 N44 C36 118.1(3) . .
C59 N51 C58 107.5(3) . .
C59 N51 C52 107.6(3) . .
C58 N51 C52 108.6(2) . .
C59 N51 Cd1 111.70(19) . .
C58 N51 Cd1 113.92(19) . .
C52 N51 Cd1 107.28(19) . .
C52 N53 C60 108.6(3) . .
C52 N53 C54 107.9(3) . .
C60 N53 C54 108.1(3) . .
C54 N55 C59 108.8(3) . .
C54 N55 C56 108.8(3) . .
C59 N55 C56 108.5(3) . .
C56 N57 C58 108.4(3) . .
C56 N57 C60 108.0(3) . .
C58 N57 C60 107.3(3) . .
O32 N20 O31 123.6(4) . .
O32 N20 C16 118.4(3) . .
O31 N20 C16 118.0(3) . .
C12 O11 Cd1 125.8(2) . .
O11 Cd1 O11 180.0 2 .
O11 Cd1 O1 88.93(9) 2 .
O11 Cd1 O1 91.07(9) . .
O11 Cd1 O1 91.07(9) 2 2
O11 Cd1 O1 88.94(9) . 2
O1 Cd1 O1 180.0 . 2
O11 Cd1 N51 89.37(9) 2 2
O11 Cd1 N51 90.63(9) . 2
O1 Cd1 N51 93.32(10) . 2
O1 Cd1 N51 86.68(10) 2 2
O11 Cd1 N51 90.63(9) 2 .
O11 Cd1 N51 89.37(9) . .
O1 Cd1 N51 86.68(10) . .
O1 Cd1 N51 93.32(10) 2 .
N51 Cd1 N51 180.0 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C52 N53 1.467(5) .
C52 N51 1.490(4) .
C54 N55 1.460(4) .
C54 N53 1.484(5) .
C56 N55 1.463(5) .
C56 N57 1.478(4) .
C58 N57 1.483(4) .
C58 N51 1.489(4) .
C59 N55 1.461(5) .
C59 N51 1.484(4) .
C60 N53 1.478(4) .
C60 N57 1.489(4) .
C12 O13 1.258(4) .
C12 O11 1.266(4) .
C12 C14 1.506(4) .
C14 C15 1.390(5) .
C14 C19 1.400(5) .
C15 C16 1.368(4) .
C16 C17 1.404(5) .
C16 N20 1.476(5) .
C17 C18 1.378(5) .
C18 C19 1.390(5) .
C31 C32 1.387(5) .
C31 C36 1.391(5) .
C32 C33 1.399(4) .
C32 C41 1.502(5) .
C33 C34 1.396(5) .
C34 C35 1.385(5) .
C35 C36 1.395(5) .
C36 N44 1.466(5) .
C41 O43 1.222(4) .
C41 O42 1.318(4) .
N44 O46 1.229(4) .
N44 O45 1.237(4) .
N51 Cd1 2.402(3) .
N20 O32 1.217(4) .
N20 O31 1.238(4) .
O11 Cd1 2.234(2) .
Cd1 O11 2.234(2) 2
Cd1 O1 2.301(3) .
Cd1 O1 2.301(3) 2
Cd1 N51 2.402(3) 2
