#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/43/2014343.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_2014343
loop_
_publ_author_name
'Cheng, Mei-Ling'
'Li, Hong-Xi'
'Zhang Yong'
'Lang, Jian-Ping'
_publ_section_title
;Dichloro[(3,5-dimethyl-1H-pyrazol-1-yl)methane]zinc(II) and
 di-μ-chloro-bis{chloro[(3,5-dimethyl-1H-pyrazol-1-yl)methane]cadmium(II)}
;
_journal_coeditor_code           GD1428
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m74
_journal_page_last               m77
_journal_paper_doi               10.1107/S0108270106001387
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd2 (C11 H16 N4)2 Cl4]'
_chemical_formula_moiety         'C22 H32 Cd2 Cl4 N8'
_chemical_formula_sum            'C22 H32 Cd2 Cl4 N8'
_chemical_formula_weight         775.16
_chemical_name_systematic
;
Di-μ-chloro-bis{chloro[(3,5-dimethyl-1H-pyrazol-1-yl)methane]cadmium(II)}
;
_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           SHELXL97
_cell_angle_alpha                112.752(19)
_cell_angle_beta                 102.34(2)
_cell_angle_gamma                97.28(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7033(17)
_cell_length_b                   9.232(2)
_cell_length_c                   11.513(2)
_cell_measurement_reflns_used    3251
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.3
_cell_volume                     717.4(3)
_computing_cell_refinement       'Crystal Clear'
_computing_data_collection       'Crystal Clear (Rigaku, 2001)'
_computing_data_reduction        'Crystal Structure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976) and SHELXL97'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7007
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.444
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0177
_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)+(0.0223P)²+0.3284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                2487
_reflns_number_total             2597
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd1428.cif
_cod_data_source_block           II
_cod_database_code               2014343
_cod_database_fobs_code          2014343
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Cd1 0.075656(19) 0.473155(16) 0.158421(13) 0.01859(6) Uani d . 1 . . Cd
Cl1 0.21178(7) 0.45855(7) -0.01992(5) 0.02577(12) Uani d . 1 . . Cl
Cl2 0.09753(7) 0.70804(6) 0.36282(5) 0.02550(12) Uani d . 1 . . Cl
N1 -0.0949(2) 0.2317(2) 0.12488(16) 0.0202(4) Uani d . 1 . . N
N2 -0.0813(2) 0.1883(2) 0.22764(16) 0.0192(4) Uani d . 1 . . N
N3 0.2331(2) 0.3085(2) 0.35230(16) 0.0196(4) Uani d . 1 . . N
N4 0.2956(2) 0.3835(2) 0.28157(16) 0.0201(4) Uani d . 1 . . N
C1 -0.2498(4) 0.1056(3) -0.1132(2) 0.0356(6) Uani d . 1 . . C
H1A -0.3317 0.1782 -0.1151 0.053 Uiso calc R 1 . . H
H1B -0.3107 -0.0039 -0.1805 0.053 Uiso calc R 1 . . H
H1C -0.1378 0.1433 -0.1308 0.053 Uiso calc R 1 . . H
C2 -0.2030(3) 0.1044(3) 0.0191(2) 0.0234(4) Uani d . 1 . . C
C3 -0.2590(3) -0.0198(3) 0.0540(2) 0.0290(5) Uani d . 1 . . C
H3 -0.3368 -0.1229 -0.0033 0.035 Uiso calc R 1 . . H
C4 -0.1800(3) 0.0359(2) 0.1867(2) 0.0235(4) Uani d . 1 . . C
C5 -0.1930(3) -0.0421(3) 0.2777(2) 0.0329(5) Uani d . 1 . . C
H5A -0.0728 -0.0581 0.3125 0.049 Uiso calc R 1 . . H
H5B -0.2810 -0.1469 0.2296 0.049 Uiso calc R 1 . . H
H5C -0.2337 0.0274 0.3505 0.049 Uiso calc R 1 . . H
C6 0.0446(3) 0.2973(2) 0.35436(19) 0.0200(4) Uani d . 1 . . C
H6A 0.0257 0.2590 0.4210 0.024 Uiso calc R 1 . . H
H6B 0.0186 0.4060 0.3803 0.024 Uiso calc R 1 . . H
C7 0.3387(3) 0.1687(3) 0.4944(2) 0.0329(5) Uani d . 1 . . C
H7A 0.2556 0.2128 0.5453 0.049 Uiso calc R 1 . . H
H7B 0.4559 0.1795 0.5544 0.049 Uiso calc R 1 . . H
H7C 0.2849 0.0543 0.4357 0.049 Uiso calc R 1 . . H
C8 0.3685(3) 0.2596(2) 0.41435(19) 0.0217(4) Uani d . 1 . . C
C9 0.5214(3) 0.3043(3) 0.3825(2) 0.0254(5) Uani d . 1 . . C
H9 0.6392 0.2876 0.4111 0.030 Uiso calc R 1 . . H
C10 0.4712(3) 0.3797(2) 0.2993(2) 0.0210(4) Uani d . 1 . . C
C11 0.5839(3) 0.4470(3) 0.2336(2) 0.0303(5) Uani d . 1 . . C
H11A 0.5940 0.3588 0.1553 0.046 Uiso calc R 1 . . H
H11B 0.7061 0.5036 0.2945 0.046 Uiso calc R 1 . . H
H11C 0.5258 0.5228 0.2079 0.046 Uiso calc R 1 . . H
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'
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'
N N 0.0061 0.0033 '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_3
_geom_angle
_geom_angle_publ_flag
N1 Cd1 N4 . 79.00(6) yes
N1 Cd1 Cl2 . 116.72(5) yes
N4 Cd1 Cl2 . 89.61(5) yes
N1 Cd1 Cl1 . 114.00(5) yes
N4 Cd1 Cl1 . 100.11(4) yes
Cl2 Cd1 Cl1 . 129.28(3) yes
N1 Cd1 Cl1 2_565 92.87(5) yes
N4 Cd1 Cl1 2_565 171.52(4) yes
Cl2 Cd1 Cl1 2_565 91.95(3) yes
Cl1 Cd1 Cl1 2_565 85.32(2) yes
Cd1 Cl1 Cd1 2_565 94.68(2) yes
C2 N1 N2 . 105.76(16) no
C2 N1 Cd1 . 134.16(14) no
N2 N1 Cd1 . 119.78(12) no
C4 N2 N1 . 111.33(16) no
C4 N2 C6 . 129.86(17) no
N1 N2 C6 . 118.42(16) no
C8 N3 N4 . 111.39(17) no
C8 N3 C6 . 130.13(17) no
N4 N3 C6 . 118.45(16) no
C10 N4 N3 . 105.62(16) no
C10 N4 Cd1 . 137.37(14) no
N3 N4 Cd1 . 116.96(12) no
C2 C1 H1A . 109.5 no
C2 C1 H1B . 109.5 no
H1A C1 H1B . 109.5 no
C2 C1 H1C . 109.5 no
H1A C1 H1C . 109.5 no
H1B C1 H1C . 109.5 no
N1 C2 C3 . 109.83(19) no
N1 C2 C1 . 121.49(19) no
C3 C2 C1 . 128.7(2) no
C4 C3 C2 . 107.09(19) no
C4 C3 H3 . 126.5 no
C2 C3 H3 . 126.5 no
N2 C4 C3 . 105.99(19) no
N2 C4 C5 . 123.1(2) no
C3 C4 C5 . 130.9(2) no
C4 C5 H5A . 109.5 no
C4 C5 H5B . 109.5 no
H5A C5 H5B . 109.5 no
C4 C5 H5C . 109.5 no
H5A C5 H5C . 109.5 no
H5B C5 H5C . 109.5 no
N2 C6 N3 . 111.93(16) no
N2 C6 H6A . 109.2 no
N3 C6 H6A . 109.2 no
N2 C6 H6B . 109.2 no
N3 C6 H6B . 109.2 no
H6A C6 H6B . 107.9 no
C8 C7 H7A . 109.5 no
C8 C7 H7B . 109.5 no
H7A C7 H7B . 109.5 no
C8 C7 H7C . 109.5 no
H7A C7 H7C . 109.5 no
H7B C7 H7C . 109.5 no
N3 C8 C9 . 106.07(18) no
N3 C8 C7 . 123.3(2) no
C9 C8 C7 . 130.6(2) no
C8 C9 C10 . 107.01(18) no
C8 C9 H9 . 126.5 no
C10 C9 H9 . 126.5 no
N4 C10 C9 . 109.91(19) no
N4 C10 C11 . 120.89(19) no
C9 C10 C11 . 129.18(19) no
C10 C11 H11A . 109.5 no
C10 C11 H11B . 109.5 no
H11A C11 H11B . 109.5 no
C10 C11 H11C . 109.5 no
H11A C11 H11C . 109.5 no
H11B C11 H11C . 109.5 no
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 N1 . 2.2847(19) yes
Cd1 N4 . 2.4088(18) yes
Cd1 Cl2 . 2.4616(9) yes
Cd1 Cl1 . 2.4649(7) yes
Cd1 Cl1 2_565 2.7322(9) yes
Cl1 Cd1 2_565 2.7322(9) yes
N1 C2 . 1.331(3) no
N1 N2 . 1.377(2) no
N2 C4 . 1.358(3) no
N2 C6 . 1.447(3) no
N3 C8 . 1.361(3) no
N3 N4 . 1.375(2) no
N3 C6 . 1.449(3) no
N4 C10 . 1.331(3) no
C1 C2 . 1.493(3) no
C1 H1A . 0.9800 no
C1 H1B . 0.9800 no
C1 H1C . 0.9800 no
C2 C3 . 1.402(3) no
C3 C4 . 1.373(3) no
C3 H3 . 0.9500 no
C4 C5 . 1.495(3) no
C5 H5A . 0.9800 no
C5 H5B . 0.9800 no
C5 H5C . 0.9800 no
C6 H6A . 0.9900 no
C6 H6B . 0.9900 no
C7 C8 . 1.498(3) no
C7 H7A . 0.9800 no
C7 H7B . 0.9800 no
C7 H7C . 0.9800 no
C8 C9 . 1.368(3) no
C9 C10 . 1.406(3) no
C9 H9 . 0.9500 no
C10 C11 . 1.489(3) no
C11 H11A . 0.9800 no
C11 H11B . 0.9800 no
C11 H11C . 0.9800 no
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
C6 H6A Cl2 2_566 0.99 2.77 3.666(2) 151
