#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007211.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_2007211
loop_
_publ_author_name
'Ward, M. D.'
'Mann, K. L. V.'
'Jeffery, J. C.'
'McCleverty, J. A.'
_publ_section_title
;
 A Dinuclear Indium(III) Complex with Two Pyrazolate Bridging Ligands
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              601
_journal_page_last               603
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety
'[In2 Cl4 (C8 H6 N3 )2 (C3 H7 N O )2 ] , 2C3 H7 N O'
_chemical_formula_sum            'C28 H40 Cl4 In2 N10 O4'
_chemical_formula_weight         952.14
_chemical_name_systematic
;
Tetrachloro-bis[3-(2-pyridyl)pyrazolato]-bis(N,N'-dimethyformamide)
diindium(III) bis(N,N'-dimethyformamide) solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.845(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.639(3)
_cell_length_b                   13.143(2)
_cell_length_c                   15.1992(14)
_cell_measurement_reflns_used    340
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3839.6(9)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART area detector'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12182
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0275
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0696
_refine_ls_wR_factor_obs         0.0643
_reflns_number_observed          3485
_reflns_number_total             4394
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    bm1206.cif
_[local]_cod_data_source_block   1
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_cod_database_code               2007211
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
In1 0.01969(11) 0.01488(10) 0.01678(10) 0.00031(9) 0.00474(7) -0.00097(8)
Cl2 0.0214(4) 0.0400(4) 0.0235(3) 0.0018(3) 0.0024(3) 0.0038(3)
O31 0.0250(11) 0.0331(12) 0.0252(10) -0.0009(10) -0.0007(9) -0.0043(9)
N21 0.0224(13) 0.0185(12) 0.0238(12) -0.0015(10) 0.0071(10) -0.0018(10)
N11 0.0208(13) 0.0153(11) 0.0179(11) -0.0003(10) 0.0065(10) -0.0006(9)
C23 0.026(2) 0.025(2) 0.027(2) -0.0033(13) 0.0103(13) 0.0013(13)
C15 0.020(2) 0.0174(13) 0.0191(13) 0.0025(11) 0.0036(12) 0.0023(11)
C25 0.040(2) 0.0153(14) 0.037(2) -0.0025(13) 0.012(2) 0.0007(12)
C22 0.0195(15) 0.0197(14) 0.0221(14) -0.0006(12) 0.0042(12) 0.0002(11)
C26 0.033(2) 0.0182(14) 0.030(2) -0.0017(13) 0.0091(14) -0.0021(12)
C24 0.031(2) 0.026(2) 0.031(2) -0.0047(14) 0.0082(14) 0.0053(13)
O41 0.075(2) 0.052(2) 0.062(2) -0.013(2) 0.043(2) -0.0104(14)
C42 0.040(2) 0.044(2) 0.044(2) -0.003(2) 0.011(2) -0.008(2)
N43 0.032(2) 0.052(2) 0.038(2) -0.0015(14) 0.0089(13) 0.0071(13)
C44 0.054(3) 0.069(3) 0.053(3) 0.013(2) 0.021(2) 0.006(2)
C45 0.074(3) 0.085(4) 0.061(3) -0.011(3) 0.030(3) 0.026(2)
Cl1 0.0430(5) 0.0196(4) 0.0334(4) 0.0014(3) 0.0171(4) -0.0064(3)
C14 0.039(2) 0.023(2) 0.027(2) 0.0037(14) 0.0203(15) 0.0017(12)
N33 0.0236(15) 0.053(2) 0.0231(13) -0.0104(13) -0.0012(11) -0.0004(12)
C32 0.029(2) 0.034(2) 0.0230(15) -0.0093(14) 0.0045(13) 0.0015(13)
C34 0.027(2) 0.077(3) 0.054(2) 0.008(2) -0.002(2) 0.002(2)
C35 0.037(2) 0.088(3) 0.043(2) -0.022(2) -0.007(2) -0.020(2)
N12 0.0287(14) 0.0139(11) 0.0195(11) 0.0010(10) 0.0084(10) -0.0015(9)
C13 0.044(2) 0.022(2) 0.027(2) 0.0070(14) 0.0216(15) -0.0019(12)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
In1 0.482967(10) 0.159116(14) 0.011166(12) 0.01697(7) Uani d . 1 In
Cl2 0.37150(4) 0.16316(6) -0.09772(5) 0.0286(2) Uani d . 1 Cl
O31 0.58865(11) 0.15584(15) 0.09960(13) 0.0286(5) Uani d . 1 O
N21 0.53069(12) 0.2721(2) -0.07367(15) 0.0212(5) Uani d . 1 N
N11 0.53585(12) 0.0672(2) -0.07778(14) 0.0177(5) Uani d . 1 N
C23 0.5884(2) 0.2906(2) -0.1969(2) 0.0253(7) Uani d . 1 C
H23 0.6102(2) 0.2601(2) -0.2407(2) 0.030 Uiso calc R 1 H
C15 0.56259(15) 0.1192(2) -0.1386(2) 0.0191(6) Uani d . 1 C
C25 0.5525(2) 0.4378(2) -0.1263(2) 0.0301(7) Uani d . 1 C
H25 0.5487(2) 0.5095(2) -0.1213(2) 0.036 Uiso calc R 1 H
C22 0.56095(15) 0.2305(2) -0.1373(2) 0.0204(6) Uani d . 1 C
C26 0.5271(2) 0.3740(2) -0.0689(2) 0.0268(7) Uani d . 1 C
H26 0.5062(2) 0.4033(2) -0.0238(2) 0.032 Uiso calc R 1 H
C24 0.5836(2) 0.3957(2) -0.1914(2) 0.0287(7) Uani d . 1 C
H24 0.6014(2) 0.4381(2) -0.2319(2) 0.034 Uiso calc R 1 H
O41 0.1312(2) 0.9647(2) 0.1422(2) 0.0588(8) Uani d . 1 O
C42 0.1551(2) 1.0223(3) 0.0949(2) 0.0423(9) Uani d . 1 C
H42 0.1393(2) 1.0907(3) 0.0920(2) 0.051 Uiso calc R 1 H
N43 0.20180(15) 0.9980(2) 0.0463(2) 0.0405(7) Uani d . 1 N
C44 0.2266(2) 0.8933(3) 0.0449(3) 0.0572(11) Uani d . 1 C
H44A 0.2605(2) 0.8889(3) 0.0059(3) 0.086 Uiso calc R 1 H
H44B 0.1872(2) 0.8483(3) 0.0218(3) 0.086 Uiso calc R 1 H
H44C 0.2486(2) 0.8724(3) 0.1060(3) 0.086 Uiso calc R 1 H
C45 0.2267(2) 1.0732(4) -0.0100(3) 0.0710(14) Uani d . 1 C
H45A 0.2606(2) 1.0416(4) -0.0406(3) 0.107 Uiso calc R 1 H
H45B 0.2488(2) 1.1296(4) 0.0276(3) 0.107 Uiso calc R 1 H
H45C 0.1874(2) 1.0992(4) -0.0548(3) 0.107 Uiso calc R 1 H
Cl1 0.44841(4) 0.29043(5) 0.10723(5) 0.0307(2) Uani d . 1 Cl
C14 0.5889(2) 0.0521(2) -0.1939(2) 0.0280(7) Uani d . 1 C
H14 0.6108(2) 0.0679(2) -0.2424(2) 0.034 Uiso calc R 1 H
N33 0.67500(14) 0.2001(2) 0.2147(2) 0.0340(6) Uani d . 1 N
C32 0.6147(2) 0.2158(2) 0.1607(2) 0.0287(7) Uani d . 1 C
H32 0.5897(2) 0.2759(2) 0.1685(2) 0.034 Uiso calc R 1 H
C34 0.7149(2) 0.1094(3) 0.2075(3) 0.0541(11) Uani d . 1 C
H34A 0.7580(2) 0.1109(3) 0.2532(3) 0.081 Uiso calc R 1 H
H34B 0.7261(2) 0.1064(3) 0.1476(3) 0.081 Uiso calc R 1 H
H34C 0.6876(2) 0.0493(3) 0.2166(3) 0.081 Uiso calc R 1 H
C35 0.7026(2) 0.2744(3) 0.2847(2) 0.0586(12) Uani d . 1 C
H35A 0.7477(2) 0.2508(3) 0.3188(2) 0.088 Uiso calc R 1 H
H35B 0.6701(2) 0.2819(3) 0.3254(2) 0.088 Uiso calc R 1 H
H35C 0.7085(2) 0.3401(3) 0.2568(2) 0.088 Uiso calc R 1 H
N12 0.54341(13) -0.0332(2) -0.09284(15) 0.0202(5) Uani d . 1 N
C13 0.5758(2) -0.0422(2) -0.1623(2) 0.0289(7) Uani d . 1 C
H13 0.5879(2) -0.1049(2) -0.1861(2) 0.035 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'
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'
In In -0.7276 1.3100 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N12 In1 N11 5_655 . 97.38(8) yes
N12 In1 O31 5_655 . 86.73(8) yes
N11 In1 O31 . . 82.12(8) yes
N12 In1 N21 5_655 . 168.38(8) yes
N11 In1 N21 . . 73.36(8) yes
O31 In1 N21 . . 85.07(8) yes
N12 In1 Cl1 5_655 . 93.88(6) yes
N11 In1 Cl1 . . 165.55(6) yes
O31 In1 Cl1 . . 89.53(6) yes
N21 In1 Cl1 . . 94.27(6) yes
N12 In1 Cl2 5_655 . 96.68(7) yes
N11 In1 Cl2 . . 93.72(6) yes
O31 In1 Cl2 . . 174.96(5) yes
N21 In1 Cl2 . . 91.02(6) yes
Cl1 In1 Cl2 . . 93.94(3) yes
C32 O31 In1 . . 128.8(2) yes
C26 N21 C22 . . 118.6(2) ?
C26 N21 In1 . . 125.7(2) ?
C22 N21 In1 . . 115.6(2) ?
C15 N11 N12 . . 108.0(2) ?
C15 N11 In1 . . 116.1(2) ?
N12 N11 In1 . . 135.6(2) ?
C24 C23 C22 . . 119.0(3) ?
N11 C15 C14 . . 109.9(2) ?
N11 C15 C22 . . 119.2(2) ?
C14 C15 C22 . . 130.8(2) ?
C26 C25 C24 . . 118.8(3) ?
N21 C22 C23 . . 121.5(3) ?
N21 C22 C15 . . 115.3(2) ?
C23 C22 C15 . . 123.2(2) ?
N21 C26 C25 . . 122.9(3) ?
C25 C24 C23 . . 119.2(3) ?
O41 C42 N43 . . 125.5(4) ?
C42 N43 C45 . . 121.1(3) ?
C42 N43 C44 . . 120.2(3) ?
C45 N43 C44 . . 118.6(3) ?
C13 C14 C15 . . 104.0(2) ?
C32 N33 C34 . . 121.1(3) ?
C32 N33 C35 . . 120.1(3) ?
C34 N33 C35 . . 118.7(3) ?
O31 C32 N33 . . 123.2(3) ?
C13 N12 N11 . . 107.7(2) ?
C13 N12 In1 . 5_655 125.7(2) ?
N11 N12 In1 . 5_655 126.4(2) ?
N12 C13 C14 . . 110.4(2) ?
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
In1 N12 5_655 2.193(2) yes
In1 N11 . 2.223(2) yes
In1 O31 . 2.230(2) yes
In1 N21 . 2.289(2) yes
In1 Cl1 . 2.4449(7) yes
In1 Cl2 . 2.4591(8) yes
O31 C32 . 1.245(3) ?
N21 C26 . 1.344(4) ?
N21 C22 . 1.351(3) ?
N11 C15 . 1.340(3) ?
N11 N12 . 1.353(3) ?
C23 C24 . 1.389(4) ?
C23 C22 . 1.391(4) ?
C15 C14 . 1.389(4) ?
C15 C22 . 1.463(4) ?
C25 C26 . 1.376(4) ?
C25 C24 . 1.380(4) ?
O41 C42 . 1.204(4) ?
C42 N43 . 1.329(4) ?
N43 C45 . 1.456(4) ?
N43 C44 . 1.462(4) ?
C14 C13 . 1.373(4) ?
N33 C32 . 1.312(4) ?
N33 C34 . 1.442(5) ?
N33 C35 . 1.464(4) ?
N12 C13 . 1.345(3) ?
N12 In1 5_655 2.193(2) ?