#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/09/2010935.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_2010935
loop_
_publ_author_name
'Huang, Wen-Tao'
'Lo, Jem-Mau'
'Yao, Hsueh-Hua'
'Liao, Fen-Ling'
_publ_section_title
μ-Oxo-bis{{2,2'-[2,2-dimethylpropane-1,3-diylbis(nitrilomethylidyne)]diphenolato}oxorhenium(V)}
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e172
_journal_page_last               e173
_journal_paper_doi               10.1107/S0108270100004455
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Re2 O3 (C19 H20 N2 O2)2]'
_chemical_formula_sum            'C38 H40 N4 O7 Re2'
_chemical_formula_weight         1037.14
_chemical_name_systematic
;
μ-oxo-bis-{oxo[N,N'-2,2-dimethylpropane-1,3-
diylbis(salicylideneiminato)]rhenium (V)}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2427(2)
_cell_length_b                   13.3736(2)
_cell_length_c                   12.4932(2)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     1785.38(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1991)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .908
_diffrn_measured_fraction_theta_max .908
_diffrn_measurement_device_type  'CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0559
_diffrn_reflns_av_sigmaI/netI    .0617
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10934
_diffrn_reflns_theta_full        28.79
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    6.830
_exptl_absorpt_correction_T_max  .664
_exptl_absorpt_correction_T_min  .274
_exptl_absorpt_correction_type
'empirical from equivalent data (Sheldrick, 1991)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tabular
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .06
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          .058
_refine_ls_R_factor_gt           .038
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0352P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .084
_reflns_number_gt                3266
_reflns_number_total             4225
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0249.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010935
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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
Re1 .048078(19) .134220(15) .546208(17) .03092(8) Uani d . 1 . . Re
O1 .0000 .0000 .5000 .0340(12) Uani d S 1 . . O
O2 .1108(4) .2492(3) .5846(4) .0454(10) Uani d . 1 . . O
O3 .0324(4) .1010(3) .6994(3) .0420(9) Uani d . 1 . . O
O4 -.1335(3) .1715(3) .5121(3) .0398(9) Uani d . 1 . . O
N1 .2294(4) .0692(3) .5884(4) .0392(11) Uani d . 1 . . N
N2 .0395(4) .1571(3) .3758(4) .0319(10) Uani d . 1 . . N
C1 .1201(6) .0645(4) .7872(5) .0392(14) Uani d . 1 . . C
C2 .0928(7) .0562(5) .8884(5) .0563(18) Uani d . 1 . . C
H2A .0147 .0764 .8912 .068 Uiso calc R 1 . . H
C3 .1783(8) .0189(6) .9844(6) .071(2) Uani d . 1 . . C
H3A .1575 .0146 1.0507 .085 Uiso calc R 1 . . H
C4 .2949(8) -.0123(6) .9829(6) .074(2) Uani d . 1 . . C
H4A .3525 -.0378 1.0477 .088 Uiso calc R 1 . . H
C5 .3247(7) -.0053(5) .8853(6) .066(2) Uani d . 1 . . C
H5A .4034 -.0266 .8853 .079 Uiso calc R 1 . . H
C6 .2409(6) .0332(4) .7839(5) .0454(15) Uani d . 1 . . C
C7 .2841(5) .0344(4) .6881(5) .0432(15) Uani d . 1 . . C
H7A .3625 .0063 .6988 .052 Uiso calc R 1 . . H
C8 .2910(5) .0462(4) .5034(5) .0438(14) Uani d . 1 . . C
H8A .2619 -.0189 .4715 .053 Uiso calc R 1 . . H
H8B .3802 .0407 .5413 .053 Uiso calc R 1 . . H
C9 .2710(5) .1206(4) .4063(6) .0422(14) Uani d . 1 . . C
C10 .1345(5) .1171(4) .3289(5) .0426(14) Uani d . 1 . . C
H10A .1293 .1540 .2607 .051 Uiso calc R 1 . . H
H10B .1135 .0480 .3074 .051 Uiso calc R 1 . . H
C11 -.0533(5) .2009(4) .3054(5) .0386(13) Uani d . 1 . . C
H11A -.0449 .2139 .2350 .046 Uiso calc R 1 . . H
C12 -.1692(5) .2328(4) .3209(5) .0343(12) Uani d . 1 . . C
C13 -.2541(6) .2796(5) .2279(5) .0506(16) Uani d . 1 . . C
H13A -.2285 .2957 .1660 .061 Uiso calc R 1 . . H
C14 -.3740(6) .3025(5) .2253(6) .0579(19) Uani d . 1 . . C
H14A -.4288 .3337 .1628 .070 Uiso calc R 1 . . H
C15 -.4115(6) .2786(5) .3164(6) .0509(17) Uani d . 1 . . C
H15A -.4930 .2926 .3148 .061 Uiso calc R 1 . . H
C16 -.3309(5) .2345(4) .4098(5) .0419(14) Uani d . 1 . . C
H16A -.3590 .2184 .4702 .050 Uiso calc R 1 . . H
C17 -.2063(5) .2129(4) .4161(5) .0331(12) Uani d . 1 . . C
C18 .3132(6) .2254(5) .4461(6) .0533(17) Uani d . 1 . . C
H18A .3984 .2237 .4942 .080 Uiso calc R 1 . . H
H18B .2608 .2517 .4872 .080 Uiso calc R 1 . . H
H18C .3071 .2673 .3823 .080 Uiso calc R 1 . . H
C19 .3479(6) .0816(5) .3330(6) .0588(18) Uani d . 1 . . C
H19A .4351 .0816 .3759 .088 Uiso calc R 1 . . H
H19B .3347 .1240 .2683 .088 Uiso calc R 1 . . H
H19C .3220 .0147 .3088 .088 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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
_geom_angle_publ_flag
O2 Re1 O1 . 171.76(14) yes
O2 Re1 O4 . 98.06(18) yes
O1 Re1 O4 . 89.75(12) yes
O2 Re1 O3 . 94.71(19) yes
O1 Re1 O3 . 88.86(12) yes
O4 Re1 O3 . 82.77(15) yes
O2 Re1 N2 . 92.19(19) yes
O1 Re1 N2 . 84.94(12) yes
O4 Re1 N2 . 91.43(16) yes
O3 Re1 N2 . 171.54(15) yes
O2 Re1 N1 . 91.05(18) yes
O1 Re1 N1 . 81.39(12) yes
O4 Re1 N1 . 169.80(16) yes
O3 Re1 N1 . 91.95(18) yes
N2 Re1 N1 . 92.80(18) yes
Re1 O1 Re1 3_556 180.0 yes
C1 O3 Re1 . 127.3(4) no
C17 O4 Re1 . 126.0(3) no
C7 N1 C8 . 115.5(5) no
C7 N1 Re1 . 121.2(4) no
C8 N1 Re1 . 122.5(4) no
C11 N2 C10 . 115.6(5) no
C11 N2 Re1 . 121.9(4) no
C10 N2 Re1 . 122.4(3) no
O3 C1 C2 . 117.7(6) no
O3 C1 C6 . 123.6(5) no
C2 C1 C6 . 118.7(6) no
C3 C2 C1 . 121.8(7) no
C2 C3 C4 . 120.4(8) no
C5 C4 C3 . 119.3(7) no
C4 C5 C6 . 122.9(7) no
C5 C6 C7 . 116.7(6) no
C5 C6 C1 . 116.9(6) no
C7 C6 C1 . 126.4(5) no
N1 C7 C6 . 129.0(6) no
N1 C8 C9 . 116.7(5) no
C18 C9 C8 . 112.9(6) no
C18 C9 C19 . 109.5(5) no
C8 C9 C19 . 106.3(5) no
C18 C9 C10 . 112.6(5) no
C8 C9 C10 . 110.5(5) no
C19 C9 C10 . 104.5(5) no
N2 C10 C9 . 116.4(5) no
N2 C11 C12 . 128.5(5) no
C13 C12 C17 . 118.8(5) no
C13 C12 C11 . 115.7(5) no
C17 C12 C11 . 125.3(5) no
C14 C13 C12 . 122.1(6) no
C15 C14 C13 . 118.8(6) no
C14 C15 C16 . 121.1(6) no
C15 C16 C17 . 121.4(6) no
O4 C17 C12 . 125.1(5) no
O4 C17 C16 . 117.0(5) no
C12 C17 C16 . 117.8(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
Re1 O2 . 1.697(4) yes
Re1 O1 . 1.9114(2) yes
Re1 O4 . 2.015(4) yes
Re1 O3 . 2.025(4) yes
Re1 N2 . 2.123(5) yes
Re1 N1 . 2.126(5) yes
O3 C1 . 1.320(6) no
O4 C17 . 1.343(6) no
N1 C7 . 1.292(7) yes
N1 C8 . 1.470(8) no
N2 C11 . 1.279(7) yes
N2 C10 . 1.469(7) no
C1 C2 . 1.395(9) no
C1 C6 . 1.434(9) no
C2 C3 . 1.376(9) no
C3 C4 . 1.381(12) no
C4 C5 . 1.364(12) no
C5 C6 . 1.420(8) no
C6 C7 . 1.425(9) no
C8 C9 . 1.530(8) no
C9 C18 . 1.514(8) no
C9 C19 . 1.534(9) no
C9 C10 . 1.540(8) no
C11 C12 . 1.439(7) no
C12 C13 . 1.401(7) no
C12 C17 . 1.404(8) no
C13 C14 . 1.377(9) no
C14 C15 . 1.368(10) no
C15 C16 . 1.369(8) no
C16 C17 . 1.407(7) no
