#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/28/2222801.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2222801
loop_
_publ_author_name
'Blake, Karyn M.'
'LaDuca, Robert L.'
_publ_section_title
;Poly[[bis[μ-1,4-bis(3-pyridylmethyl)piperazine-κ²N:N']dichloridocadmium(II)]
 tetrahydrate]
;
_journal_coeditor_code           LH2863
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m947
_journal_paper_doi               10.1107/S1600536809027767
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cd Cl2 (C16 H20 N4)2], 4H2 O'
_chemical_formula_moiety         'C32 H40 Cd Cl2 N8, 4(H2 O)'
_chemical_formula_sum            'C32 H48 Cd Cl2 N8 O4'
_chemical_formula_weight         792.08
_chemical_name_systematic
;
Poly[[bis[μ-1,4-bis(3-pyridylmethyl)piperazine-
κ²N:N']dichloridocadmium(II)] tetrahydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.4730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3481(2)
_cell_length_b                   13.9791(2)
_cell_length_c                   12.7789(2)
_cell_measurement_reflns_used    16643
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.16
_cell_volume                     1846.84(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ'
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0261P)²+0.7641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                3060
_reflns_number_total             3391
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2863.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2222801
_cod_database_fobs_code          2222801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd1 0.0000 0.5000 0.5000 0.01972(7) Uani d S 1 . .
Cl Cl1 -0.00576(4) 0.56521(3) 0.69090(3) 0.02753(11) Uani d . 1 . .
O O1W 0.31111(17) 1.01315(12) 0.44201(15) 0.0498(4) Uani d D 1 . .
H H1WA 0.267(2) 0.9840(17) 0.3915(18) 0.060 Uiso d D 1 . .
H H1WB 0.375(2) 1.0362(19) 0.4063(19) 0.060 Uiso d D 1 . .
O O2W 0.4410(2) 0.92673(13) 0.61847(14) 0.0623(5) Uani d D 1 . .
H H2WA 0.385(3) 0.958(2) 0.5722(19) 0.075 Uiso d D 1 . .
H H2WB 0.443(3) 0.9689(18) 0.6730(17) 0.075 Uiso d D 1 . .
N N1 0.16425(14) 0.61714(10) 0.46966(11) 0.0256(3) Uani d . 1 . .
N N2 0.14429(14) 0.90557(10) 0.29043(11) 0.0242(3) Uani d . 1 . .
N N3 -0.05153(14) 1.05084(11) 0.26799(11) 0.0267(3) Uani d . 1 . .
N N4 -0.35028(14) 1.12026(10) 0.05522(11) 0.0235(3) Uani d . 1 . .
C C1 0.14831(17) 0.67064(12) 0.38328(14) 0.0254(4) Uani d . 1 . .
H H1 0.0828 0.6526 0.3328 0.031 Uiso calc R 1 . .
C C2 0.22184(17) 0.75090(12) 0.36317(14) 0.0246(4) Uani d . 1 . .
C C3 0.31970(18) 0.77468(13) 0.43639(15) 0.0301(4) Uani d . 1 . .
H H3 0.3738 0.8283 0.4251 0.036 Uiso calc R 1 . .
C C4 0.33772(19) 0.71988(13) 0.52574(16) 0.0336(4) Uani d . 1 . .
H H4 0.4041 0.7354 0.5766 0.040 Uiso calc R 1 . .
C C5 0.25809(18) 0.64246(13) 0.53994(15) 0.0308(4) Uani d . 1 . .
H H5 0.2701 0.6055 0.6020 0.037 Uiso calc R 1 . .
C C6 0.19428(18) 0.80989(13) 0.26599(14) 0.0281(4) Uani d . 1 . .
H H6A 0.2748 0.8168 0.2276 0.034 Uiso calc R 1 . .
H H6B 0.1301 0.7760 0.2197 0.034 Uiso calc R 1 . .
C C7 0.02170(18) 0.90049(13) 0.34449(15) 0.0290(4) Uani d . 1 . .
H H7A 0.0356 0.8657 0.4115 0.035 Uiso calc R 1 . .
H H7B -0.0430 0.8647 0.3006 0.035 Uiso calc R 1 . .
C C8 -0.0291(2) 0.99965(13) 0.36577(16) 0.0309(4) Uani d . 1 . .
H H8A -0.1109 0.9950 0.4028 0.037 Uiso calc R 1 . .
H H8B 0.0344 1.0350 0.4112 0.037 Uiso calc R 1 . .
C C9 0.06858(18) 1.05772(13) 0.21285(15) 0.0307(4) Uani d . 1 . .
H H9A 0.1326 1.0953 0.2555 0.037 Uiso calc R 1 . .
H H9B 0.0521 1.0916 0.1456 0.037 Uiso calc R 1 . .
C C10 0.12320(18) 0.95935(14) 0.19196(14) 0.0297(4) Uani d . 1 . .
H H10A 0.0624 0.9237 0.1444 0.036 Uiso calc R 1 . .
H H10B 0.2062 0.9659 0.1569 0.036 Uiso calc R 1 . .
C C11 -0.11128(18) 1.14457(13) 0.28181(15) 0.0312(4) Uani d . 1 . .
H H11A -0.0434 1.1930 0.2976 0.037 Uiso calc R 1 . .
H H11B -0.1691 1.1423 0.3415 0.037 Uiso calc R 1 . .
C C12 -0.27629(17) 1.10601(12) 0.14168(14) 0.0247(4) Uani d . 1 . .
H H12 -0.2843 1.0468 0.1772 0.030 Uiso calc R 1 . .
C C13 -0.18808(16) 1.17228(12) 0.18317(14) 0.0243(4) Uani d . 1 . .
C C14 -0.17827(18) 1.25856(13) 0.13158(15) 0.0298(4) Uani d . 1 . .
H H14 -0.1203 1.3064 0.1578 0.036 Uiso calc R 1 . .
C C15 -0.25411(18) 1.27477(13) 0.04085(15) 0.0311(4) Uani d . 1 . .
H H15 -0.2482 1.3335 0.0040 0.037 Uiso calc R 1 . .
C C16 -0.33791(17) 1.20436(12) 0.00536(14) 0.0261(4) Uani d . 1 . .
H H16 -0.3892 1.2156 -0.0569 0.031 Uiso calc R 1 . .
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 Cd1 N4 4_676 2_445 180.0 ?
N4 Cd1 N1 4_676 . 94.21(5) ?
N4 Cd1 N1 2_445 . 85.79(5) ?
N4 Cd1 N1 4_676 3_566 85.79(5) ?
N4 Cd1 N1 2_445 3_566 94.21(5) ?
N1 Cd1 N1 . 3_566 180.00(5) ?
N4 Cd1 Cl1 4_676 . 90.60(4) ?
N4 Cd1 Cl1 2_445 . 89.40(4) ?
N1 Cd1 Cl1 . . 87.57(4) ?
N1 Cd1 Cl1 3_566 . 92.43(4) ?
N4 Cd1 Cl1 4_676 3_566 89.40(4) ?
N4 Cd1 Cl1 2_445 3_566 90.60(4) ?
N1 Cd1 Cl1 . 3_566 92.43(4) ?
N1 Cd1 Cl1 3_566 3_566 87.57(4) ?
Cl1 Cd1 Cl1 . 3_566 180.0 ?
H1WA O1W H1WB . . 100(2) ?
H2WA O2W H2WB . . 100(2) ?
C1 N1 C5 . . 117.70(16) ?
C1 N1 Cd1 . . 116.82(11) ?
C5 N1 Cd1 . . 124.63(12) ?
C7 N2 C6 . . 111.94(14) ?
C7 N2 C10 . . 109.05(14) ?
C6 N2 C10 . . 108.82(14) ?
C8 N3 C9 . . 109.92(14) ?
C8 N3 C11 . . 113.01(15) ?
C9 N3 C11 . . 111.90(15) ?
C12 N4 C16 . . 117.41(15) ?
C12 N4 Cd1 . 2_455 119.03(11) ?
C16 N4 Cd1 . 2_455 123.53(11) ?
N1 C1 C2 . . 123.82(16) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C1 C2 C3 . . 117.32(16) ?
C1 C2 C6 . . 120.65(16) ?
C3 C2 C6 . . 122.03(16) ?
C4 C3 C2 . . 119.52(17) ?
C4 C3 H3 . . 120.2 ?
C2 C3 H3 . . 120.2 ?
C5 C4 C3 . . 118.99(18) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N1 C5 C4 . . 122.63(18) ?
N1 C5 H5 . . 118.7 ?
C4 C5 H5 . . 118.7 ?
N2 C6 C2 . . 112.20(14) ?
N2 C6 H6A . . 109.2 ?
C2 C6 H6A . . 109.2 ?
N2 C6 H6B . . 109.2 ?
C2 C6 H6B . . 109.2 ?
H6A C6 H6B . . 107.9 ?
N2 C7 C8 . . 110.71(15) ?
N2 C7 H7A . . 109.5 ?
C8 C7 H7A . . 109.5 ?
N2 C7 H7B . . 109.5 ?
C8 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
N3 C8 C7 . . 109.98(16) ?
N3 C8 H8A . . 109.7 ?
C7 C8 H8A . . 109.7 ?
N3 C8 H8B . . 109.7 ?
C7 C8 H8B . . 109.7 ?
H8A C8 H8B . . 108.2 ?
N3 C9 C10 . . 110.96(15) ?
N3 C9 H9A . . 109.4 ?
C10 C9 H9A . . 109.4 ?
N3 C9 H9B . . 109.4 ?
C10 C9 H9B . . 109.4 ?
H9A C9 H9B . . 108.0 ?
N2 C10 C9 . . 110.80(15) ?
N2 C10 H10A . . 109.5 ?
C9 C10 H10A . . 109.5 ?
N2 C10 H10B . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 108.1 ?
N3 C11 C13 . . 109.80(14) ?
N3 C11 H11A . . 109.7 ?
C13 C11 H11A . . 109.7 ?
N3 C11 H11B . . 109.7 ?
C13 C11 H11B . . 109.7 ?
H11A C11 H11B . . 108.2 ?
N4 C12 C13 . . 124.16(16) ?
N4 C12 H12 . . 117.9 ?
C13 C12 H12 . . 117.9 ?
C14 C13 C12 . . 117.45(16) ?
C14 C13 C11 . . 125.13(16) ?
C12 C13 C11 . . 117.42(16) ?
C13 C14 C15 . . 119.35(16) ?
C13 C14 H14 . . 120.3 ?
C15 C14 H14 . . 120.3 ?
C16 C15 C14 . . 118.91(17) ?
C16 C15 H15 . . 120.5 ?
C14 C15 H15 . . 120.5 ?
N4 C16 C15 . . 122.71(16) ?
N4 C16 H16 . . 118.6 ?
C15 C16 H16 . . 118.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cd1 N4 4_676 2.3728(14) ?
Cd1 N4 2_445 2.3728(14) ?
Cd1 N1 . 2.4036(15) ?
Cd1 N1 3_566 2.4036(15) ?
Cd1 Cl1 . 2.6074(4) ?
Cd1 Cl1 3_566 2.6074(4) ?
O1W H1WA . 0.874(16) ?
O1W H1WB . 0.884(16) ?
O2W H2WA . 0.921(17) ?
O2W H2WB . 0.912(17) ?
N1 C1 . 1.338(2) ?
N1 C5 . 1.342(2) ?
N2 C7 . 1.472(2) ?
N2 C6 . 1.472(2) ?
N2 C10 . 1.474(2) ?
N3 C8 . 1.450(2) ?
N3 C9 . 1.458(2) ?
N3 C11 . 1.463(2) ?
N4 C12 . 1.332(2) ?
N4 C16 . 1.346(2) ?
N4 Cd1 2_455 2.3728(14) ?
C1 C2 . 1.386(2) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.389(3) ?
C2 C6 . 1.508(2) ?
C3 C4 . 1.381(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.377(3) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.511(3) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.515(3) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C13 . 1.511(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.390(2) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.380(3) ?
C14 C15 . 1.390(3) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.376(3) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1WA N2 . 0.874(16) 2.084(17) 2.950(2) 171(2) y
O1W H1WB O2W 3_676 0.884(16) 2.007(18) 2.838(3) 156(2) y
O2W H2WA O1W . 0.921(17) 1.958(19) 2.844(3) 161(3) y
O2W H2WB Cl1 2_556 0.912(17) 2.272(18) 3.1607(17) 165(3) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N4 Cd1 N1 C1 4_676 . . . 138.25(13) ?
N4 Cd1 N1 C1 2_445 . . . -41.75(13) ?
Cl1 Cd1 N1 C1 . . . . -131.32(12) ?
Cl1 Cd1 N1 C1 3_566 . . . 48.68(12) ?
N4 Cd1 N1 C5 4_676 . . . -52.61(14) ?
N4 Cd1 N1 C5 2_445 . . . 127.39(14) ?
Cl1 Cd1 N1 C5 . . . . 37.82(14) ?
Cl1 Cd1 N1 C5 3_566 . . . -142.18(14) ?
C5 N1 C1 C2 . . . . -0.8(3) ?
Cd1 N1 C1 C2 . . . . 169.09(13) ?
N1 C1 C2 C3 . . . . 1.8(3) ?
N1 C1 C2 C6 . . . . -177.44(16) ?
C1 C2 C3 C4 . . . . -1.5(3) ?
C6 C2 C3 C4 . . . . 177.80(17) ?
C2 C3 C4 C5 . . . . 0.2(3) ?
C1 N1 C5 C4 . . . . -0.6(3) ?
Cd1 N1 C5 C4 . . . . -169.62(14) ?
C3 C4 C5 N1 . . . . 0.9(3) ?
C7 N2 C6 C2 . . . . -60.88(19) ?
C10 N2 C6 C2 . . . . 178.52(15) ?
C1 C2 C6 N2 . . . . 112.33(18) ?
C3 C2 C6 N2 . . . . -66.9(2) ?
C6 N2 C7 C8 . . . . -178.39(15) ?
C10 N2 C7 C8 . . . . -57.93(19) ?
C9 N3 C8 C7 . . . . -59.1(2) ?
C11 N3 C8 C7 . . . . 175.07(15) ?
N2 C7 C8 N3 . . . . 60.0(2) ?
C8 N3 C9 C10 . . . . 58.00(19) ?
C11 N3 C9 C10 . . . . -175.57(14) ?
C7 N2 C10 C9 . . . . 56.28(19) ?
C6 N2 C10 C9 . . . . 178.64(15) ?
N3 C9 C10 N2 . . . . -57.0(2) ?
C8 N3 C11 C13 . . . . -153.02(16) ?
C9 N3 C11 C13 . . . . 82.25(18) ?
C16 N4 C12 C13 . . . . 0.1(3) ?
Cd1 N4 C12 C13 2_455 . . . -178.06(13) ?
N4 C12 C13 C14 . . . . 0.7(3) ?
N4 C12 C13 C11 . . . . -179.79(16) ?
N3 C11 C13 C14 . . . . -129.54(18) ?
N3 C11 C13 C12 . . . . 51.0(2) ?
C12 C13 C14 C15 . . . . -1.0(3) ?
C11 C13 C14 C15 . . . . 179.54(18) ?
C13 C14 C15 C16 . . . . 0.5(3) ?
C12 N4 C16 C15 . . . . -0.7(3) ?
Cd1 N4 C16 C15 2_455 . . . 177.39(14) ?
C14 C15 C16 N4 . . . . 0.4(3) ?
