#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:31:37 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179583 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/48/4504840.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_4504840
loop_
_publ_author_name
'Thorn, Adrienne'
'Willett, Roger D.'
'Twamley, Brendan'
_publ_section_title
;
 Retro-Crystal Engineering Analysis of TwoN-Methylethylenediammonium
 Cadmium Halide Salts Obtained by Dimensional Reduction and Recombination
 of the Hexagonal CdX2Lattice
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              673
_journal_paper_doi               10.1021/cg030059s
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C3 H16 Cd2 Cl6 N2 O2'
_chemical_formula_weight         549.68
_chemical_name_systematic
; 
 Bis(N-methylethylenediammonium hydrate)dodecachloro-
Tetracadmate(II) dihydrate
;
_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                106.402(2)
_cell_angle_beta                 97.426(2)
_cell_angle_gamma                107.732(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7129(8)
_cell_length_b                   9.6624(11)
_cell_length_c                   13.4553(16)
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.53
_cell_volume                     775.01(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      303(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  '‘CCD area detector’'
_diffrn_measurement_method       '‘phi and omega’'
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7144
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.35
_diffrn_standards_interval_time  '&#x0091;beginning and edn&#x0092;'
_diffrn_standards_number         '&#x0091;50 frames&#x0092;'
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_type   &#x0091;empirical&#x0092;
_exptl_absorpt_process_details   ‘SADABS’
_exptl_crystal_colour            &#x0091;colorless&#x0092;
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ‘needle’
_exptl_crystal_F_000             524
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0307
_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 
 [0.00000+1.00000exp(1.50(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.4659*P+(0.0317P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                1992
_reflns_number_total             2709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg030059s_s1.cif
_cod_data_source_block           p1b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504840
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
Cd1 Cd 0.60766(6) -0.17087(4) -0.24219(3) 0.03691(15) Uani 1 1 d . . .
Cd2 Cd 0.20341(6) -0.05298(4) -0.08371(3) 0.03332(14) Uani 1 1 d . . .
Cl1 Cl 0.6167(2) -0.43322(16) -0.33673(12) 0.0504(4) Uani 1 1 d . . .
Cl2 Cl 1.0042(2) -0.00449(15) -0.23828(11) 0.0385(3) Uani 1 1 d . . .
Cl3 Cl 0.2346(2) -0.29794(14) -0.20226(10) 0.0378(3) Uani 1 1 d . . .
Cl4 Cl 0.60457(19) 0.08989(13) -0.09217(10) 0.0322(3) Uani 1 1 d . . .
Cl5 Cl -0.18516(19) -0.19553(13) -0.05383(10) 0.0329(3) Uani 1 1 d . . .
Cl6 Cl 0.4611(3) -0.1041(2) -0.39669(13) 0.0602(4) Uani 1 1 d . . .
N1 N -0.0360(8) -0.3072(5) -0.4588(4) 0.0526(13) Uani 1 1 d . A 1
H1C H 0.1000 -0.2504 -0.4211 0.063 Uiso 1 1 calc R A 1
H1D H -0.1183 -0.3238 -0.4125 0.063 Uiso 1 1 calc R A 1
C1 C -0.0427(10) -0.4572(7) -0.5301(5) 0.0522(16) Uani 1 1 d . . 1
H1A H 0.0417 -0.4395 -0.5817 0.063 Uiso 1 1 calc R . 1
H1B H -0.1901 -0.5197 -0.5689 0.063 Uiso 1 1 calc R . 1
C2 C -0.114(2) -0.2209(15) -0.5197(11) 0.061(4) Uani 0.50 1 d P A 1
H2A H -0.1068 -0.1240 -0.4715 0.092 Uiso 0.50 1 calc PR A 1
H2B H -0.2600 -0.2803 -0.5587 0.092 Uiso 0.50 1 calc PR A 1
H2C H -0.0252 -0.2021 -0.5686 0.092 Uiso 0.50 1 calc PR A 1
O1 O 0.7295(14) 0.2795(9) -0.2906(6) 0.145(3) Uani 1 1 d . B 1
O2 O -0.224(3) -0.1467(16) -0.5643(12) 0.132(5) Uani 0.50 1 d P C 2
O3 O 1.4081(17) 0.3983(13) -0.1765(10) 0.088(4) Uani 0.50 1 d P D 3
N2 N 1.0050(19) 0.3582(11) -0.1224(8) 0.049(3) Uiso 0.50 1 d PD . 4
N3 N 0.8981(18) 0.6292(11) 0.1116(8) 0.044(3) Uiso 0.50 1 d PD . 4
C3 C 1.044(2) 0.4972(15) -0.0294(10) 0.065(4) Uiso 0.50 1 d PD . 4
C4 C 0.8488(19) 0.4869(16) 0.0109(11) 0.062(4) Uiso 0.50 1 d PD . 4
C5 C 0.692(3) 0.613(2) 0.1471(16) 0.083(6) Uiso 0.50 1 d PD . 4
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'
Cd Cd -0.8075 1.2024 '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'
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
Cl6 Cd1 Cl1 101.15(6) . .
Cl6 Cd1 Cl3 96.46(5) . .
Cl1 Cd1 Cl3 90.93(4) . .
Cl6 Cd1 Cl2 90.65(5) . .
Cl1 Cd1 Cl2 97.79(5) . .
Cl3 Cd1 Cl2 167.49(4) . .
Cl6 Cd1 Cl4 93.55(5) . .
Cl1 Cd1 Cl4 164.54(5) . .
Cl3 Cd1 Cl4 82.63(4) . .
Cl2 Cd1 Cl4 86.69(4) . .
Cl6 Cd1 Cl5 170.85(5) . 1_655
Cl1 Cd1 Cl5 86.14(5) . 1_655
Cl3 Cd1 Cl5 88.86(4) . 1_655
Cl2 Cd1 Cl5 82.82(4) . 1_655
Cl4 Cd1 Cl5 79.72(4) . 1_655
Cl3 Cd2 Cl2 94.09(4) . 1_455
Cl3 Cd2 Cl5 174.92(4) . 2
Cl2 Cd2 Cl5 90.95(4) 1_455 2
Cl3 Cd2 Cl4 86.31(4) . .
Cl2 Cd2 Cl4 98.53(4) 1_455 .
Cl5 Cd2 Cl4 93.55(4) 2 .
Cl3 Cd2 Cl5 95.20(4) . .
Cl2 Cd2 Cl5 87.30(4) 1_455 .
Cl5 Cd2 Cl5 84.42(4) 2 .
Cl4 Cd2 Cl5 173.87(4) . .
Cl3 Cd2 Cl4 90.72(4) . 2_655
Cl2 Cd2 Cl4 174.58(4) 1_455 2_655
Cl5 Cd2 Cl4 84.21(4) 2 2_655
Cl4 Cd2 Cl4 84.26(4) . 2_655
Cl5 Cd2 Cl4 89.77(4) . 2_655
Cd2 Cl2 Cd1 98.33(5) 1_655 .
Cd2 Cl3 Cd1 97.98(4) . .
Cd2 Cl4 Cd2 95.74(4) . 2_655
Cd2 Cl4 Cd1 92.14(4) . .
Cd2 Cl4 Cd1 98.08(4) 2_655 .
Cd2 Cl5 Cd2 95.58(4) 2 .
Cd2 Cl5 Cd1 97.97(4) 2 1_455
Cd2 Cl5 Cd1 90.69(4) . 1_455
C1 N1 C2 111.4(7) . .
N1 C1 C1 111.9(6) . 2_544
N3 N2 C4 64.6(14) 2_765 2_765
N3 N2 C3 88.1(17) 2_765 .
C4 N2 C3 23.5(7) 2_765 .
N3 N2 C5 21.9(15) 2_765 2_765
C4 N2 C5 80.5(8) 2_765 2_765
C3 N2 C5 102.5(9) . 2_765
N2 N3 C4 94.3(16) 2_765 .
N2 N3 C3 69.1(15) 2_765 2_765
C4 N3 C3 25.3(7) . 2_765
N2 N3 C5 149(2) 2_765 .
C4 N3 C5 106.7(11) . .
C3 N3 C5 128.6(11) 2_765 .
C4 C3 C3 114(3) 2_765 2_765
C4 C3 C4 139.6(19) 2_765 .
C3 C3 C4 25.3(12) 2_765 .
C4 C3 N3 74.3(16) 2_765 2_765
C3 C3 N3 138(2) 2_765 2_765
C4 C3 N3 131.0(10) . 2_765
C4 C3 N2 97.0(18) 2_765 .
C3 C3 N2 125.4(18) 2_765 .
C4 C3 N2 110.8(9) . .
N3 C3 N2 22.8(5) 2_765 .
C3 C4 C3 40.4(19) 2_765 .
C3 C4 C4 27.8(13) 2_765 2_765
C3 C4 C4 12.6(7) . 2_765
C3 C4 N3 80.4(17) 2_765 .
C3 C4 N3 109.5(9) . .
C4 C4 N3 100.6(10) 2_765 .
C3 C4 N2 59.5(15) 2_765 2_765
C3 C4 N2 90.1(9) . 2_765
C4 C4 N2 80.2(8) 2_765 2_765
N3 C4 N2 21.0(5) . 2_765
N2 C5 N3 8.8(6) 2_765 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 Cl6 2.5142(16) .
Cd1 Cl1 2.5181(14) .
Cd1 Cl3 2.6300(13) .
Cd1 Cl2 2.6424(14) .
Cd1 Cl4 2.7557(13) .
Cd1 Cl5 2.8366(13) 1_655
Cd2 Cl3 2.5389(13) .
Cd2 Cl2 2.5587(14) 1_455
Cd2 Cl5 2.6332(12) 2
Cd2 Cl4 2.6597(13) .
Cd2 Cl5 2.6940(13) .
Cd2 Cl4 2.7124(13) 2_655
Cl2 Cd2 2.5587(14) 1_655
Cl4 Cd2 2.7124(13) 2_655
Cl5 Cd2 2.6332(12) 2
Cl5 Cd1 2.8366(13) 1_455
N1 C1 1.479(7) .
N1 C2 1.478(14) .
C1 C1 1.489(12) 2_544
N2 N3 0.614(13) 2_765
N2 C4 1.706(18) 2_765
N2 C3 1.480(10) .
N2 C5 2.049(16) 2_765
N3 N2 0.614(13) 2_765
N3 C4 1.546(15) .
N3 C3 1.583(16) 2_765
N3 C5 1.496(11) .
C3 C4 0.686(19) 2_765
C3 C3 1.04(2) 2_765
C3 C4 1.466(10) .
C3 N3 1.583(16) 2_765
C4 C3 0.686(19) 2_765
C4 C4 2.04(2) 2_765
C4 N2 1.706(18) 2_765
C5 N2 2.049(16) 2_765
