#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2215128.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_2215128
loop_
_publ_author_name
'Chun-Fang Huang'
'Hua-Long Chen'
_publ_section_title
;\
catena-Poly[[chloridonickel(II)]-di-\m-chlorido-[chloridonickel(II)]-\m-\
4,4'-methylenebis(3,5-dimethylpyrazole)-\k^2^N^2^:N^2'^]
;
_journal_coeditor_code HB2501
_journal_issue 9
_journal_name_full 'Acta Crystallographica, Section E'
_journal_page_first m2356
_journal_page_last m2357
_journal_volume 63
_journal_year 2007
_chemical_formula_iupac '[Ni Cl2 (C11 H16 N4)]'
_chemical_formula_moiety 'C11 H16 Cl2 N4 Ni'
_chemical_formula_sum 'C11 H16 Cl2 N4 Ni'
_chemical_formula_weight 333.89
_chemical_name_systematic
;
catena-Poly[[chloridonickel(II)]-di-\m-chlorido-[chloridonickel(II)]-\m-\
4,4'-methylenebis(3,5-dimethylpyrazole)-\k^2^N^2^:N^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 79.269(6)
_cell_angle_beta 63.584(5)
_cell_angle_gamma 86.922(5)
_cell_formula_units_Z 2
_cell_length_a 8.759(3)
_cell_length_b 8.879(3)
_cell_length_c 9.735(3)
_cell_measurement_reflns_used 3212
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 25.10
_cell_measurement_theta_min 2.34
_cell_volume 665.8(4)
_computing_cell_refinement 'SAINT (Bruker, 1999)'
_computing_data_collection 'APEX2 (Bruker, 1998)'
_computing_data_reduction SAINT
_computing_molecular_graphics 'SHELXTL (Bruker, 1998)'
_computing_publication_material SHELXTL
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type 'Bruker APEX II CCD'
_diffrn_measurement_method \w
_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 0.0327
_diffrn_reflns_av_sigmaI/netI 0.0853
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 3330
_diffrn_reflns_theta_full 25.10
_diffrn_reflns_theta_max 25.10
_diffrn_reflns_theta_min 2.34
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.845
_exptl_absorpt_correction_T_max 0.769
_exptl_absorpt_correction_T_min 0.626
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.665
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 344
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.728
_refine_diff_density_min -1.047
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.974
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 169
_refine_ls_number_reflns 2312
_refine_ls_number_restraints 40
_refine_ls_restrained_S_all 0.980
_refine_ls_R_factor_all 0.0911
_refine_ls_R_factor_gt 0.0654
_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 w=1/[\s^2^(Fo^2^)+(0.1397P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1861
_refine_ls_wR_factor_ref 0.2083
_reflns_number_gt 1534
_reflns_number_total 2312
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file hb2501.cif
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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'
Ni Ni 0.3393 1.1124 '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_
_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
Ni Ni2 0.36689(12) 0.08445(11) 0.90152(10) 0.0275(4) Uani d . 1
Cl Cl1 0.1129(2) 0.0033(2) 1.1136(2) 0.0370(5) Uani d . 1
Cl Cl2 0.4813(3) -0.1538(2) 0.9274(2) 0.0384(6) Uani d . 1
C C8 0.6764(9) 0.5680(8) 0.1917(8) 0.0277(16) Uani d . 1
N N2 0.8976(7) 0.7132(6) 0.1257(7) 0.0324(15) Uani d D 1
C C10 0.9389(9) 0.5714(9) 0.1731(8) 0.0299(17) Uani d . 1
C C3 0.7286(9) 0.2395(8) 0.4362(8) 0.0295(17) Uani d . 1
N N4 0.7209(8) 0.1467(8) 0.6655(7) 0.0371(17) Uani d . 1
N N3 0.5559(8) 0.1395(8) 0.6870(7) 0.0373(16) Uani d . 1
C C4 0.8261(10) 0.2016(10) 0.5168(9) 0.039(2) Uani d . 1
C C6 0.7886(10) 0.3010(9) 0.2662(8) 0.0339(19) Uani d . 1
H H39A 0.7122 0.2606 0.2331 0.041 Uiso calc RU 1
H H39B 0.9005 0.2615 0.2101 0.041 Uiso calc RU 1
C C7 0.8005(9) 0.4745(8) 0.2170(8) 0.0289(17) Uani d . 1
C C1 0.4016(10) 0.1983(10) 0.5276(9) 0.042(2) Uani d . 1
H H1C 0.3209 0.1224 0.6070 0.063 Uiso calc RU 1
H H1A 0.4272 0.1766 0.4267 0.063 Uiso calc RU 1
H H1B 0.3538 0.2979 0.5364 0.063 Uiso calc RU 1
C C2 0.5595(10) 0.1951(8) 0.5472(9) 0.0306(17) Uani d . 1
C C5 1.0141(10) 0.2126(12) 0.4657(10) 0.049(2) Uani d . 1
H H45A 1.0450 0.3135 0.4691 0.074 Uiso calc RU 1
H H45B 1.0742 0.1934 0.3611 0.074 Uiso calc RU 1
H H45C 1.0438 0.1380 0.5342 0.074 Uiso calc RU 1
C C9 0.5025(10) 0.5253(9) 0.2176(10) 0.041(2) Uani d . 1
H H30A 0.4218 0.5337 0.3219 0.061 Uiso calc RU 1
H H30B 0.5007 0.4215 0.2028 0.061 Uiso calc RU 1
H H30C 0.4728 0.5929 0.1446 0.061 Uiso calc RU 1
C C11 1.1094(10) 0.5454(11) 0.1706(10) 0.045(2) Uani d . 1
H H47A 1.1901 0.6217 0.0919 0.068 Uiso calc RU 1
H H47B 1.1461 0.4453 0.1477 0.068 Uiso calc RU 1
H H47C 1.1020 0.5524 0.2706 0.068 Uiso calc RU 1
N N1 0.7387(7) 0.7146(6) 0.1358(7) 0.0348(16) Uani d . 1
H H4 0.7577 0.1015 0.7460 0.070(6) Uiso d RU 1
H H2 0.9769 0.7979 0.0653 0.069(6) Uiso d RDU 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni2 0.0317(6) 0.0230(6) 0.0266(6) 0.0017(4) -0.0143(4) 0.0015(4)
Cl1 0.0349(11) 0.0368(12) 0.0387(11) -0.0040(9) -0.0201(9) 0.0060(9)
Cl2 0.0499(13) 0.0277(11) 0.0434(12) 0.0046(9) -0.0264(10) -0.0058(9)
C8 0.033(4) 0.022(4) 0.024(4) 0.004(3) -0.011(3) 0.000(3)
N2 0.029(3) 0.026(4) 0.039(4) -0.001(3) -0.016(3) 0.005(3)
C10 0.029(4) 0.033(4) 0.026(4) -0.001(3) -0.011(3) -0.003(3)
C3 0.033(4) 0.020(4) 0.033(4) 0.001(3) -0.014(3) -0.001(3)
N4 0.032(4) 0.044(4) 0.038(4) -0.004(3) -0.022(3) 0.003(3)
N3 0.036(4) 0.038(4) 0.035(4) 0.009(3) -0.017(3) -0.001(3)
C4 0.045(5) 0.039(5) 0.030(4) 0.005(4) -0.019(4) 0.003(4)
C6 0.041(5) 0.028(4) 0.031(4) 0.012(4) -0.017(4) -0.003(3)
C7 0.035(4) 0.023(4) 0.030(4) 0.002(3) -0.016(3) -0.004(3)
C1 0.048(5) 0.044(5) 0.037(5) 0.005(4) -0.023(4) -0.003(4)
C2 0.036(4) 0.023(4) 0.036(4) 0.003(3) -0.021(4) -0.002(3)
C5 0.041(5) 0.064(7) 0.046(5) 0.003(5) -0.027(4) 0.000(5)
C9 0.038(5) 0.031(5) 0.065(6) -0.007(4) -0.032(4) -0.008(4)
C11 0.040(5) 0.047(6) 0.046(5) 0.013(4) -0.019(4) -0.006(4)
N1 0.032(4) 0.031(4) 0.039(4) -0.001(3) -0.016(3) 0.002(3)
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
Ni2 N3 . 1.992(6) y
Ni2 N1 2_666 2.013(6) y
Ni2 Cl1 . 2.294(2) y
Ni2 Cl2 . 2.311(2) y
Ni2 Cl2 2_657 2.713(2) y
Cl2 Ni2 2_657 2.713(2) ?
C8 N1 . 1.355(9) ?
C8 C7 . 1.413(10) ?
C8 C9 . 1.488(10) ?
N2 C10 . 1.346(9) ?
N2 N1 . 1.351(7) ?
N2 H2 . 0.9600 ?
C10 C7 . 1.381(10) ?
C10 C11 . 1.489(10) ?
C3 C4 . 1.387(11) ?
C3 C2 . 1.413(10) ?
C3 C6 . 1.494(10) ?
N4 C4 . 1.334(9) ?
N4 N3 . 1.369(8) ?
N4 H4 . 0.9864 ?
N3 C2 . 1.346(9) ?
C4 C5 . 1.497(11) ?
C6 C7 . 1.520(10) ?
C6 H39A . 0.9700 ?
C6 H39B . 0.9700 ?
C1 C2 . 1.476(10) ?
C1 H1C . 0.9600 ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C5 H45A . 0.9600 ?
C5 H45B . 0.9600 ?
C5 H45C . 0.9600 ?
C9 H30A . 0.9600 ?
C9 H30B . 0.9600 ?
C9 H30C . 0.9600 ?
C11 H47A . 0.9600 ?
C11 H47B . 0.9600 ?
C11 H47C . 0.9600 ?
N1 Ni2 2_666 2.013(6) ?
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
N3 Ni2 N1 . 2_666 88.6(2)
N3 Ni2 Cl1 . . 164.9(2)
N1 Ni2 Cl1 2_666 . 88.90(16)
N3 Ni2 Cl2 . . 89.5(2)
N1 Ni2 Cl2 2_666 . 174.54(19)
Cl1 Ni2 Cl2 . . 91.59(8)
N3 Ni2 Cl2 . 2_657 100.5(2)
N1 Ni2 Cl2 2_666 2_657 100.84(19)
Cl1 Ni2 Cl2 . 2_657 94.60(8)
Cl2 Ni2 Cl2 . 2_657 84.54(8)
Ni2 Cl2 Ni2 . 2_657 95.46(8)
N1 C8 C7 . . 109.2(7)
N1 C8 C9 . . 121.4(6)
C7 C8 C9 . . 129.4(7)
C10 N2 N1 . . 111.6(4)
C10 N2 H2 . . 125.4
N1 N2 H2 . . 120.8
N2 C10 C7 . . 107.3(6)
N2 C10 C11 . . 120.0(7)
C7 C10 C11 . . 132.7(8)
C4 C3 C2 . . 105.0(7)
C4 C3 C6 . . 128.1(7)
C2 C3 C6 . . 126.7(7)
C4 N4 N3 . . 111.0(6)
C4 N4 H4 . . 124.8
N3 N4 H4 . . 123.5
C2 N3 N4 . . 106.1(6)
C2 N3 Ni2 . . 133.1(5)
N4 N3 Ni2 . . 120.0(5)
N4 C4 C3 . . 108.0(7)
N4 C4 C5 . . 119.9(7)
C3 C4 C5 . . 132.0(7)
C3 C6 C7 . . 116.8(6)
C3 C6 H39A . . 108.1
C7 C6 H39A . . 108.1
C3 C6 H39B . . 108.1
C7 C6 H39B . . 108.1
H39A C6 H39B . . 107.3
C10 C7 C8 . . 105.6(7)
C10 C7 C6 . . 127.7(7)
C8 C7 C6 . . 126.4(7)
C2 C1 H1C . . 109.5
C2 C1 H1A . . 109.5
H1C C1 H1A . . 109.5
C2 C1 H1B . . 109.5
H1C C1 H1B . . 109.5
H1A C1 H1B . . 109.5
N3 C2 C3 . . 109.7(6)
N3 C2 C1 . . 120.3(7)
C3 C2 C1 . . 129.9(7)
C4 C5 H45A . . 109.5
C4 C5 H45B . . 109.5
H45A C5 H45B . . 109.5
C4 C5 H45C . . 109.5
H45A C5 H45C . . 109.5
H45B C5 H45C . . 109.5
C8 C9 H30A . . 109.5
C8 C9 H30B . . 109.5
H30A C9 H30B . . 109.5
C8 C9 H30C . . 109.5
H30A C9 H30C . . 109.5
H30B C9 H30C . . 109.5
C10 C11 H47A . . 109.5
C10 C11 H47B . . 109.5
H47A C11 H47B . . 109.5
C10 C11 H47C . . 109.5
H47A C11 H47C . . 109.5
H47B C11 H47C . . 109.5
N2 N1 C8 . . 106.2(5)
N2 N1 Ni2 . 2_666 119.9(3)
C8 N1 Ni2 . 2_666 133.3(5)
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
N2 H2 Cl1 1_664 0.96 2.45 3.227(6) 138
N2 H2 Cl1 2_666 0.96 2.59 3.123(6) 116
N4 H4 Cl1 2_657 0.99 2.19 3.167(7) 169
_cod_database_code 2215128