#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/67/2006763.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_2006763
loop_
_publ_author_name
'Lawson, Yvonne G.'
'Norman, Nicholas C.'
'Orpen, A. Guy'
'Quayle, Michael J.'
_publ_section_title
;
 Mononuclear Indium and Gallium Tetrachlorocatecholate Complexes
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1805
_journal_page_last               1809
_journal_paper_doi               10.1107/S0108270197010901
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[In Cl (C6 Cl4 O2) (C5 H5 N1)], 2C4 H10 O'
_chemical_formula_moiety         'C29 H35 Cl5 In N3 O4'
_chemical_formula_structural     'In Cl py~2~ O~2~C~6~Cl~4~'
_chemical_formula_sum            'C29 H35 Cl5 In N3 O4'
_chemical_formula_weight         781.67
_chemical_name_systematic
;
Tetrachlorocatecholatochlorotripyridyl indium(III) diethylether solvate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.876(3)
_cell_length_b                   14.756(2)
_cell_length_c                   13.541(2)
_cell_measurement_reflns_used    192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     3372.0(9)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 60
_diffrn_measured_fraction_theta_max 99.6
_diffrn_measurement_device       'Siemens SMART area detector'
_diffrn_measurement_method       'ω rotation 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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15255
_diffrn_reflns_theta_full        49.42
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type
'empirical, pseudo-azimuthal scan (SHELXTL; Sheldrick, 1995)'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.167
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_obs          .0456
_refine_ls_shift/esd_max         -0.014
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0476P)²+8.18P] where P=[Max(Fo²,0)+2Fc²]/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1213
_refine_ls_wR_factor_obs         .1062
_reflns_number_observed          2459
_reflns_number_total             3095
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1155.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0476P)^2^+8.18P] where P=[Max(Fo^2^,0)+2Fc^2^]/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0476P)^2^+8.18P] where P=[Max(Fo^2^,0)+2Fc^2^]/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3372.2(8)
_cod_database_code               2006763
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_disorder_group
_atom_site_type_symbol
In1 .55929(3) .2500 .10468(4) .0282(2) Uani d S 1 . In
O1 .5669(3) .2500 -.0521(3) .0293(10) Uani d S 1 . O
O2 .6839(3) .2500 .0847(3) .0315(11) Uani d S 1 . O
N1 .5631(3) .0931(3) .1127(3) .0348(9) Uani d . 1 . N
N2 .5906(4) .2500 .2688(4) .0341(14) Uani d S 1 . N
Cl1 .58883(10) .2500 -.26827(13) .0364(4) Uani d S 1 . Cl
Cl2 .76733(12) .2500 -.33359(14) .0477(5) Uani d S 1 . Cl
Cl3 .90028(12) .2500 -.1745(2) .0579(6) Uani d S 1 . Cl
Cl4 .85215(12) .2500 .0511(2) .0581(6) Uani d S 1 . Cl
Cl5 .41678(11) .2500 .1223(2) .0441(5) Uani d S 1 . Cl
C1 .6417(4) .2500 -.0822(5) .0265(15) Uani d S 1 . C
C2 .6631(4) .2500 -.1808(5) .030(2) Uani d S 1 . C
C3 .7425(4) .2500 -.2097(5) .031(2) Uani d S 1 . C
C4 .8012(4) .2500 -.1394(6) .036(2) Uani d S 1 . C
C5 .7803(4) .2500 -.0393(5) .035(2) Uani d S 1 . C
C6 .7028(4) .2500 -.0096(5) .0276(15) Uani d S 1 . C
C7 .5013(4) .0440(4) .1382(5) .0500(15) Uani d . 1 . C
H7 .4542(4) .0741(4) .1581(5) .060 Uiso calc R 1 . H
C8 .5022(4) -.0499(4) .1370(5) .056(2) Uani d . 1 . C
H8 .4568(4) -.0832(4) .1573(5) .067 Uiso calc R 1 . H
C9 .5673(4) -.0930(4) .1072(4) .054(2) Uani d . 1 . C
H9 .5689(4) -.1574(4) .1056(4) .065 Uiso calc R 1 . H
C10 .6317(5) -.0436(4) .0790(5) .063(2) Uani d . 1 . C
H10 .6785(5) -.0729(4) .0565(5) .075 Uiso calc R 1 . H
C11 .6277(4) .0496(4) .0837(5) .051(2) Uani d . 1 . C
H11 .6729(4) .0839(4) .0654(5) .062 Uiso calc R 1 . H
C12 .6662(5) .2500 .2969(6) .045(2) Uani d S 1 . C
H12 .7060(5) .2500 .2474(6) .054 Uiso calc SR 1 . H
C13 .6893(5) .2500 .3945(6) .054(2) Uani d S 1 . C
H13 .7439(5) .2500 .4115(6) .065 Uiso calc SR 1 . H
C14 .6327(6) .2500 .4659(7) .072(3) Uani d S 1 . C
H14 .6469(6) .2500 .5338(7) .087 Uiso calc SR 1 . H
C15 .5548(6) .2500 .4379(7) .091(4) Uani d S 1 . C
H15 .5142(6) .2500 .4865(7) .109 Uiso calc SR 1 . H
C16 .5356(5) .2500 .3392(6) .061(3) Uani d S 1 . C
H16 .4813(5) .2500 .3207(6) .073 Uiso calc SR 1 . H
O3 .8189(5) -.0039(6) -.0373(7) .132(3) Uiso d . 1 . O
C20 .8825(12) -.0009(16) .1060(15) .241(10) Uiso d . 1 . C
H20A .9322(12) .0033(16) .1432(15) .362 Uiso calc PR .50 . H
H20B .8561(12) -.0583(16) .1213(15) .362 Uiso calc PR .50 . H
H20C .8478(12) .0497(16) .1244(15) .362 Uiso calc PR .50 . H
H20D .8252(12) -.0069(16) .1161(15) .362 Uiso calc PR .50 . H
H20E .9013(12) .0547(16) .1379(15) .362 Uiso calc PR .50 . H
H20F .9096(12) -.0533(16) .1349(15) .362 Uiso calc PR .50 . H
C21 .9004(10) .0036(11) -.0061(15) .198(7) Uani d . 1 . C
H21A .9249(10) .0618(11) -.0260(15) .238 Uiso calc R 1 . H
H21B .9334(10) -.0477(11) -.0291(15) .238 Uiso calc R 1 . H
C22 .8132(8) .0007(8) -.1420(10) .133(4) Uani d . 1 . C
H22A .8449(8) -.0494(8) -.1705(10) .160 Uiso calc R 1 . H
H22B .8374(8) .0583(8) -.1642(10) .160 Uiso calc R 1 . H
C23 .7309(7) -.0048(9) -.1828(12) .179(7) Uani d . 1 . C
H23A .7329(7) -.0011(9) -.2550(12) .268 Uiso calc PR .50 . H
H23B .6992(7) .0455(9) -.1569(12) .268 Uiso calc PR .50 . H
H23C .7067(7) -.0624(9) -.1632(12) .268 Uiso calc PR .50 . H
H23D .6929(7) -.0109(9) -.1284(12) .268 Uiso calc PR .50 . H
H23E .7266(7) -.0575(9) -.2265(12) .268 Uiso calc PR .50 . H
H23F .7191(7) .0505(9) -.2202(12) .268 Uiso calc PR .50 . 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'
O O 0.0106 0.0060 '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'
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
O2 In1 O1 . . 79.2(2) y
O2 In1 N2 . . 83.9(2) y
O1 In1 N2 . . 163.1(2) y
O2 In1 N1 . 7_565 88.75(11) ?
O1 In1 N1 . 7_565 92.60(10) ?
N2 In1 N1 . 7_565 87.00(10) ?
O2 In1 N1 . . 88.76(11) y
O1 In1 N1 . . 92.60(10) y
N2 In1 N1 . . 87.00(10) y
N1 In1 N1 7_565 . 173.7(2) y
O2 In1 Cl5 . . 178.32(13) y
O1 In1 Cl5 . . 99.12(13) y
N2 In1 Cl5 . . 97.7(2) y
N1 In1 Cl5 7_565 . 91.33(11) ?
N1 In1 Cl5 . . 91.33(11) y
C1 O1 In1 . . 111.4(4) ?
C6 O2 In1 . . 111.4(4) ?
C7 N1 C11 . . 117.5(5) ?
C7 N1 In1 . . 122.7(4) ?
C11 N1 In1 . . 119.6(4) ?
C12 N2 C16 . . 117.6(7) ?
C12 N2 In1 . . 120.0(5) ?
C16 N2 In1 . . 122.3(5) ?
C2 Cl1 Cl3 . 6 150.3(3) ?
C4 Cl3 Cl1 . 6_655 177.9(3) ?
O1 C1 C2 . . 123.1(6) ?
O1 C1 C6 . . 118.4(6) ?
C2 C1 C6 . . 118.5(6) ?
C1 C2 C3 . . 121.4(6) ?
C1 C2 Cl1 . . 118.2(5) ?
C3 C2 Cl1 . . 120.3(5) ?
C4 C3 C2 . . 119.9(7) ?
C4 C3 Cl2 . . 119.9(5) ?
C2 C3 Cl2 . . 120.3(5) ?
C3 C4 C5 . . 119.3(7) ?
C3 C4 Cl3 . . 120.3(6) ?
C5 C4 Cl3 . . 120.4(6) ?
C6 C5 C4 . . 121.6(7) ?
C6 C5 Cl4 . . 117.7(6) ?
C4 C5 Cl4 . . 120.7(6) ?
O2 C6 C5 . . 121.1(6) ?
O2 C6 C1 . . 119.6(6) ?
C5 C6 C1 . . 119.3(6) ?
N1 C7 C8 . . 122.7(6) ?
C9 C8 C7 . . 119.3(6) ?
C8 C9 C10 . . 119.1(6) ?
C9 C10 C11 . . 118.8(7) ?
N1 C11 C10 . . 122.6(6) ?
N2 C12 C13 . . 123.1(8) ?
C14 C13 C12 . . 118.9(8) ?
C13 C14 C15 . . 118.6(8) ?
C14 C15 C16 . . 119.7(9) ?
N2 C16 C15 . . 122.1(8) ?
C22 O3 C21 . . 110.6(12) ?
O3 C21 C20 . . 95.6(15) ?
O3 C22 C23 . . 115.3(12) ?
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 O2 . 2.120(5) yes
In1 O1 . 2.126(5) yes
In1 N2 . 2.284(6) yes
In1 N1 7_565 2.318(4) ?
In1 N1 . 2.318(4) yes
In1 Cl5 . 2.417(2) yes
O1 C1 . 1.327(8) yes
O2 C6 . 1.316(8) yes
N1 C7 . 1.316(7) ?
N1 C11 . 1.325(7) ?
N2 C12 . 1.330(10) ?
N2 C16 . 1.332(10) ?
Cl1 C2 . 1.724(7) ?
Cl1 Cl3 6 3.275(3) ?
Cl2 C3 . 1.729(7) ?
Cl3 C4 . 1.738(7) ?
Cl3 Cl1 6_655 3.275(3) ?
Cl4 C5 . 1.722(7) ?
C1 C2 . 1.383(9) ?
C1 C6 . 1.425(9) yes
C2 C3 . 1.397(10) ?
C3 C4 . 1.374(10) ?
C4 C5 . 1.402(10) ?
C5 C6 . 1.369(10) ?
C7 C8 . 1.385(8) ?
C8 C9 . 1.334(9) ?
C9 C10 . 1.363(9) ?
C10 C11 . 1.378(8) ?
C12 C13 . 1.378(11) ?
C13 C14 . 1.360(12) ?
C14 C15 . 1.368(13) ?
C15 C16 . 1.376(13) ?
O3 C22 . 1.422(14) ?
O3 C21 . 1.44(2) ?
C20 C21 . 1.55(2) ?
C22 C23 . 1.50(2) ?
