#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:34:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179413 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/10/4331079.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_4331079
loop_
_publ_author_name
'Lakshmi Kanta Das'
'Ramakant M. Kadam'
'Antonio Bauzá'
'Antonio Frontera'
'Ashutosh Ghosh'
_publ_section_title
;
 Differences in Nuclearity, Molecular Shapes, and Coordination Modes of
 Azide in the Complexes of Cd(II) and Hg(II) with a "Metalloligand" [CuL]
 (H2L =N,N'-Bis(salicylidene)-1,3-propanediamine): Characterization in
 Solid and in Solutions, and Theoretical Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12407
_journal_page_last               12418
_journal_paper_doi               10.1021/ic301773h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C34 H32 Cu2 Hg N10 O4'
_chemical_formula_weight         972.37
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.893(5)
_cell_angle_beta                 65.495(5)
_cell_angle_gamma                76.198(5)
_cell_formula_units_Z            1
_cell_length_a                   9.488(5)
_cell_length_b                   9.937(5)
_cell_length_c                   10.299(5)
_cell_measurement_reflns_used    11421
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.11
_cell_volume                     858.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX V1.80.03'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11421
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    5.746
_exptl_absorpt_correction_T_max  0.3928
_exptl_absorpt_correction_T_min  0.2071
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_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)+(0.0698P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                3793
_reflns_number_total             4834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301773h_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4331079
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7046(6) 0.2109(4) 0.3898(5) 0.0572(10) Uani 1 1 d . A .
C2 C 0.8385(8) 0.2382(6) 0.2748(6) 0.0751(14) Uani 1 1 d . . .
H2 H 0.9370 0.1781 0.2529 0.090 Uiso 1 1 calc R . .
C3 C 0.8239(11) 0.3552(7) 0.1934(8) 0.095(2) Uani 1 1 d . . .
H3 H 0.9138 0.3737 0.1180 0.114 Uiso 1 1 calc R . .
C4 C 0.6778(11) 0.4454(6) 0.2223(8) 0.090(2) Uani 1 1 d . . .
H4 H 0.6695 0.5223 0.1652 0.108 Uiso 1 1 calc R . .
C5 C 0.5498(9) 0.4209(6) 0.3321(7) 0.0807(18) Uani 1 1 d . . .
H5 H 0.4529 0.4834 0.3524 0.097 Uiso 1 1 calc R . .
C6 C 0.5556(7) 0.3049(4) 0.4180(6) 0.0629(12) Uani 1 1 d . . .
C7 C 0.4110(6) 0.2845(5) 0.5332(6) 0.0675(13) Uani 1 1 d . A .
H7 H 0.3201 0.3513 0.5419 0.081 Uiso 1 1 calc R . .
C8A C 0.2209(7) 0.2000(8) 0.7272(9) 0.095(2) Uani 0.44(2) 1 d P A 1
H8A1 H 0.1575 0.2911 0.7224 0.114 Uiso 0.44(2) 1 calc PR A 1
H8A2 H 0.1770 0.1312 0.7044 0.114 Uiso 0.44(2) 1 calc PR A 1
C9A C 0.219(2) 0.1768(17) 0.8694(17) 0.085(5) Uiso 0.44(2) 1 d P A 1
H9A1 H 0.2731 0.2422 0.8822 0.102 Uiso 0.44(2) 1 calc PR A 1
H9A2 H 0.1083 0.2047 0.9358 0.102 Uiso 0.44(2) 1 calc PR A 1
C10A C 0.2772(9) 0.0534(11) 0.9151(8) 0.124(3) Uani 0.44(2) 1 d P A 1
H10A H 0.2024 -0.0047 0.9328 0.149 Uiso 0.44(2) 1 calc PR A 1
H10B H 0.2774 0.0696 1.0065 0.149 Uiso 0.44(2) 1 calc PR A 1
C8B C 0.2209(7) 0.2000(8) 0.7272(9) 0.095(2) Uani 0.56(2) 1 d P A 2
H8B1 H 0.1837 0.2905 0.7729 0.114 Uiso 0.56(2) 1 calc PR A 2
H8B2 H 0.1596 0.1989 0.6719 0.114 Uiso 0.56(2) 1 calc PR A 2
C9B C 0.1795(15) 0.0977(13) 0.8404(13) 0.082(4) Uiso 0.56(2) 1 d P A 2
H9B1 H 0.0731 0.1355 0.9100 0.098 Uiso 0.56(2) 1 calc PR A 2
H9B2 H 0.1747 0.0162 0.7986 0.098 Uiso 0.56(2) 1 calc PR A 2
C10B C 0.2772(9) 0.0534(11) 0.9151(8) 0.124(3) Uani 0.56(2) 1 d P A 2
H10C H 0.2255 -0.0025 0.9951 0.149 Uiso 0.56(2) 1 calc PR A 2
H10D H 0.2888 0.1340 0.9532 0.149 Uiso 0.56(2) 1 calc PR A 2
C11 C 0.4787(7) -0.1444(6) 0.8767(6) 0.0728(13) Uani 1 1 d . A .
H11 H 0.4060 -0.1656 0.9653 0.087 Uiso 1 1 calc R . .
C12 C 0.6219(6) -0.2467(5) 0.8168(5) 0.0586(10) Uani 1 1 d . . .
C13 C 0.6375(8) -0.3721(6) 0.8882(7) 0.0761(14) Uani 1 1 d . . .
H13 H 0.5554 -0.3840 0.9748 0.091 Uiso 1 1 calc R . .
C14 C 0.7667(9) -0.4761(6) 0.8363(8) 0.0840(17) Uani 1 1 d . . .
H14 H 0.7729 -0.5592 0.8850 0.101 Uiso 1 1 calc R . .
C15 C 0.8916(8) -0.4570(6) 0.7080(8) 0.0821(16) Uani 1 1 d . . .
H15 H 0.9819 -0.5279 0.6718 0.098 Uiso 1 1 calc R . .
C16 C 0.8832(7) -0.3342(5) 0.6337(7) 0.0740(14) Uani 1 1 d . . .
H16 H 0.9675 -0.3237 0.5482 0.089 Uiso 1 1 calc R . .
C17 C 0.7466(5) -0.2244(4) 0.6873(5) 0.0533(9) Uani 1 1 d . A .
N1 N 0.3896(5) 0.1892(4) 0.6240(5) 0.0631(10) Uani 1 1 d . . .
N2 N 0.4360(5) -0.0278(5) 0.8263(5) 0.0681(10) Uani 1 1 d . . .
N11 N 0.9074(5) 0.1335(6) 0.6745(6) 0.0841(14) Uani 1 1 d . . .
N12 N 0.7691(5) 0.1863(4) 0.7172(4) 0.0626(9) Uani 1 1 d . . .
N13 N 0.6386(6) 0.2413(6) 0.7655(6) 0.0875(15) Uani 1 1 d . . .
O1 O 0.7196(4) 0.0996(3) 0.4663(4) 0.0616(8) Uani 1 1 d . . .
O2 O 0.7418(4) -0.1093(3) 0.6176(4) 0.0644(8) Uani 1 1 d . . .
Cu1 Cu 0.56372(6) 0.04068(5) 0.63719(6) 0.05208(14) Uani 1 1 d . A .
Hg1 Hg 1.0000 0.0000 0.5000 0.05943(12) Uani 1 2 d S . .
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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_3
O1 C1 C2 119.3(5) .
O1 C1 C6 122.6(5) .
C2 C1 C6 118.1(5) .
C3 C2 C1 119.8(6) .
C3 C2 H2 120.1 .
C1 C2 H2 120.1 .
C4 C3 C2 121.3(7) .
C4 C3 H3 119.3 .
C2 C3 H3 119.3 .
C5 C4 C3 119.4(6) .
C5 C4 H4 120.3 .
C3 C4 H4 120.3 .
C4 C5 C6 122.3(6) .
C4 C5 H5 118.9 .
C6 C5 H5 118.9 .
C5 C6 C1 119.1(6) .
C5 C6 C7 118.9(5) .
C1 C6 C7 122.1(4) .
N1 C7 C6 129.4(4) .
N1 C7 H7 115.3 .
C6 C7 H7 115.3 .
C9A C8A N1 107.8(8) .
C9A C8A H8A1 110.1 .
N1 C8A H8A1 110.1 .
C9A C8A H8A2 110.1 .
N1 C8A H8A2 110.1 .
H8A1 C8A H8A2 108.5 .
C10A C9A C8A 124.1(13) .
C10A C9A H9A1 106.3 .
C8A C9A H9A1 106.3 .
C10A C9A H9A2 106.3 .
C8A C9A H9A2 106.3 .
H9A1 C9A H9A2 106.4 .
C9A C10A N2 120.2(9) .
C9A C10A H10A 107.3 .
N2 C10A H10A 107.3 .
C9A C10A H10B 107.3 .
N2 C10A H10B 107.3 .
H10A C10A H10B 106.9 .
C9B C8B N1 120.3(7) .
C9B C8B H8B1 107.3 .
N1 C8B H8B1 107.3 .
C9B C8B H8B2 107.3 .
N1 C8B H8B2 107.3 .
H8B1 C8B H8B2 106.9 .
C10B C9B C8B 119.2(10) .
C10B C9B H9B1 107.5 .
C8B C9B H9B1 107.5 .
C10B C9B H9B2 107.5 .
C8B C9B H9B2 107.5 .
H9B1 C9B H9B2 107.0 .
C9B C10B N2 113.4(8) .
C9B C10B H10C 108.9 .
N2 C10B H10C 108.9 .
C9B C10B H10D 108.9 .
N2 C10B H10D 108.9 .
H10C C10B H10D 107.7 .
N2 C11 C12 129.1(5) .
N2 C11 H11 115.5 .
C12 C11 H11 115.5 .
C13 C12 C17 119.9(5) .
C13 C12 C11 118.6(5) .
C17 C12 C11 121.4(4) .
C14 C13 C12 122.4(6) .
C14 C13 H13 118.8 .
C12 C13 H13 118.8 .
C13 C14 C15 118.8(5) .
C13 C14 H14 120.6 .
C15 C14 H14 120.6 .
C16 C15 C14 121.2(5) .
C16 C15 H15 119.4 .
C14 C15 H15 119.4 .
C15 C16 C17 120.3(6) .
C15 C16 H16 119.8 .
C17 C16 H16 119.8 .
O2 C17 C12 123.1(4) .
O2 C17 C16 119.6(4) .
C12 C17 C16 117.3(4) .
C7 N1 C8B 114.5(5) .
C7 N1 C8A 114.5(5) .
C8B N1 C8A 0.0(7) .
C7 N1 Cu1 123.7(4) .
C8B N1 Cu1 121.7(4) .
C8A N1 Cu1 121.7(4) .
C11 N2 C10A 115.4(5) .
C11 N2 C10B 115.4(5) .
C10A N2 C10B 0.0(9) .
C11 N2 Cu1 124.0(3) .
C10A N2 Cu1 120.4(5) .
C10B N2 Cu1 120.4(5) .
N12 N11 Hg1 116.6(4) .
N13 N12 N11 174.9(5) .
C1 O1 Cu1 129.3(3) .
C17 O2 Cu1 129.5(3) .
O2 Cu1 O1 81.32(14) .
O2 Cu1 N1 170.58(18) .
O1 Cu1 N1 92.49(17) .
O2 Cu1 N2 90.74(17) .
O1 Cu1 N2 169.06(18) .
N1 Cu1 N2 96.27(19) .
N11 Hg1 N11 180.000(1) 2_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.314(6) .
C1 C2 1.396(8) .
C1 C6 1.426(7) .
C2 C3 1.386(9) .
C2 H2 0.9300 .
C3 C4 1.388(12) .
C3 H3 0.9300 .
C4 C5 1.329(11) .
C4 H4 0.9300 .
C5 C6 1.394(8) .
C5 H5 0.9300 .
C6 C7 1.439(8) .
C7 N1 1.261(7) .
C7 H7 0.9300 .
C8A C9A 1.454(18) .
C8A N1 1.494(8) .
C8A H8A1 0.9700 .
C8A H8A2 0.9700 .
C9A C10A 1.350(18) .
C9A H9A1 0.9700 .
C9A H9A2 0.9700 .
C10A N2 1.472(7) .
C10A H10A 0.9700 .
C10A H10B 0.9700 .
C8B C9B 1.465(14) .
C8B N1 1.494(8) .
C8B H8B1 0.9700 .
C8B H8B2 0.9700 .
C9B C10B 1.407(15) .
C9B H9B1 0.9700 .
C9B H9B2 0.9700 .
C10B N2 1.472(7) .
C10B H10C 0.9700 .
C10B H10D 0.9700 .
C11 N2 1.273(7) .
C11 C12 1.420(8) .
C11 H11 0.9300 .
C12 C13 1.398(7) .
C12 C17 1.411(7) .
C13 C14 1.344(9) .
C13 H13 0.9300 .
C14 C15 1.396(10) .
C14 H14 0.9300 .
C15 C16 1.385(8) .
C15 H15 0.9300 .
C16 C17 1.419(7) .
C16 H16 0.9300 .
C17 O2 1.297(5) .
N1 Cu1 1.978(4) .
N2 Cu1 1.981(4) .
N11 N12 1.193(6) .
N11 Hg1 2.078(5) .
N12 N13 1.137(6) .
O1 Cu1 1.923(3) .
O2 Cu1 1.920(3) .
Hg1 N11 2.078(5) 2_756
