#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/02/2220257.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_2220257
loop_
_publ_author_name
'Schutte, Marietjie'
'Visser, Hendrik G.'
'Roodt, Andreas'
_publ_section_title
;
 Aquatricarbonyl(3,5,7-tribromotropolonato)rhenium(I) methanol solvate
;
_journal_coeditor_code           KJ2103
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1610
_journal_page_last               m1611
_journal_paper_doi               10.1107/S1600536808038737
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Re (C7 H2 Br3 O2) (C O)3 (H2 O)], C H4 O'
_chemical_formula_moiety         'C10 H4 Br3 O6 Re, C H4 O'
_chemical_formula_sum            'C11 H8 Br3 O7 Re'
_chemical_formula_weight         678.1
_chemical_name_systematic
;
Aquatricarbonyl(3,5,7-tribromotropolonato)rhenium(I) methanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                109.569(5)
_cell_angle_beta                 94.285(5)
_cell_angle_gamma                102.133(5)
_cell_formula_units_Z            2
_cell_length_a                   9.090(5)
_cell_length_b                   9.379(5)
_cell_length_c                   10.010(5)
_cell_measurement_reflns_used    3145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.223
_cell_measurement_theta_min      2.194
_cell_volume                     776.3(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics
'DIAMOND (Brandenberg & Putz, 2005) and ORTEP-3 (Farrugia, 1999)'
_computing_publication_material  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8673
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.576
_exptl_absorpt_correction_T_max  0.6261
_exptl_absorpt_correction_T_min  0.1496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.405
_refine_diff_density_min         -2.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0385P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                3018
_reflns_number_total             3599
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kj2103.cif
_cod_data_source_block           I
_cod_database_code               2220257
_cod_database_fobs_code          2220257
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Re Re01 0.54228(3) 0.51098(3) 0.75340(3) 0.00853(8) Uani d . 1
Br Br1 0.46576(7) 0.05513(7) 0.28520(6) 0.01185(14) Uani d . 1
O O4 0.3428(5) 0.3587(5) 0.7724(4) 0.0107(9) Uani d . 1
C C11 0.3852(7) 0.1903(7) 0.5557(7) 0.0098(13) Uani d . 1
C C2 0.7128(8) 0.6389(7) 0.7149(7) 0.0141(8) Uani d . 1
C C15 0.1120(7) -0.0432(8) 0.6174(7) 0.0130(13) Uani d . 1
H H15 0.0347 -0.093 0.6543 0.016(19) Uiso calc R 1
C C3 0.5502(8) 0.6908(8) 0.9164(7) 0.0141(8) Uani d . 1
C C17 0.2988(7) 0.2213(7) 0.6772(6) 0.0079(12) Uani d . 1
O O5 0.4976(5) 0.3042(5) 0.5642(4) 0.0096(9) Uani d . 1
C C16 0.1735(7) 0.1137(7) 0.6939(6) 0.0100(13) Uani d . 1
C C12 0.3491(7) 0.0514(7) 0.4343(6) 0.0084(12) Uani d . 1
C C13 0.2524(7) -0.0921(7) 0.4077(7) 0.0101(13) Uani d . 1
H H13 0.2554 -0.1698 0.3217 0.012(18) Uiso calc R 1
C C14 0.1514(7) -0.1368(7) 0.4909(7) 0.0135(13) Uani d . 1
Br Br2 0.04885(8) -0.35228(8) 0.42285(7) 0.01741(15) Uani d . 1
Br Br3 0.08290(7) 0.19489(8) 0.85829(7) 0.01438(15) Uani d . 1
O O2 0.8201(5) 0.7193(5) 0.6960(5) 0.0181(11) Uani d . 1
O O3 0.5530(6) 0.8006(6) 1.0157(5) 0.0191(11) Uani d . 1
O O1 0.7678(6) 0.4158(6) 0.9272(5) 0.0221(11) Uani d . 1
C C1 0.6804(8) 0.4526(8) 0.8620(7) 0.0153(14) Uani d . 1
O O7 0.1793(6) 0.6493(6) 0.8032(5) 0.0186(11) Uani d . 1
H H7 0.1438 0.5913 0.8449 0.028 Uiso calc R 1
C C4 0.1962(8) 0.8155(7) 0.8974(7) 0.0141(8) Uani d . 1
H H4C 0.2448 0.833 0.992 0.021 Uiso calc R 1
H H4A 0.0974 0.8365 0.9024 0.021 Uiso calc R 1
H H4B 0.2572 0.8837 0.8583 0.021 Uiso calc R 1
O O6 0.3692(6) 0.5548(6) 0.6216(5) 0.0214(11) Uani d . 1
H H6A 0.295(9) 0.599(9) 0.681(8) 0.032 Uiso d . 1
H H6B 0.406(9) 0.640(9) 0.575(8) 0.032 Uiso d . 1
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 '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
_geom_angle_publ_flag
C1 Re01 C3 89.5(3) ?
C1 Re01 C2 87.8(3) ?
C3 Re01 C2 85.0(3) ?
C1 Re01 O4 96.2(2) ?
C3 Re01 O4 99.6(2) ?
C2 Re01 O4 173.9(2) ?
C1 Re01 O5 96.7(2) ?
C3 Re01 O5 171.5(2) ?
C2 Re01 O5 100.9(2) ?
O4 Re01 O5 74.07(16) y
C1 Re01 O6 174.3(3) ?
C3 Re01 O6 94.2(2) ?
C2 Re01 O6 96.8(2) ?
O4 Re01 O6 78.93(19) y
O5 Re01 O6 79.17(18) y
C17 O4 Re01 118.0(4) ?
O5 C11 C12 120.1(5) ?
O5 C11 C17 115.0(5) ?
C12 C11 C17 124.9(6) ?
O2 C2 Re01 177.7(6) ?
C16 C15 C14 128.0(6) ?
C16 C15 H15 116 ?
C14 C15 H15 116 ?
O3 C3 Re01 179.1(6) ?
O4 C17 C16 119.0(5) ?
O4 C17 C11 115.4(6) ?
C16 C17 C11 125.5(6) ?
C11 O5 Re01 117.1(4) ?
C15 C16 C17 131.3(6) ?
C15 C16 Br3 113.9(5) ?
C17 C16 Br3 114.6(4) ?
C13 C12 C11 131.5(6) ?
C13 C12 Br1 113.1(4) ?
C11 C12 Br1 115.2(5) ?
C12 C13 C14 128.9(6) ?
C12 C13 H13 115.6 ?
C14 C13 H13 115.6 ?
C13 C14 C15 128.3(6) ?
C13 C14 Br2 115.9(5) ?
C15 C14 Br2 115.8(5) ?
O1 C1 Re01 178.7(6) ?
C4 O7 H7 109.5 ?
O7 C4 H4C 109.5 ?
O7 C4 H4A 109.5 ?
H4C C4 H4A 109.5 ?
O7 C4 H4B 109.5 ?
H4C C4 H4B 109.5 ?
H4A C4 H4B 109.5 ?
Re01 O6 H6A 110(4) ?
Re01 O6 H6B 117(4) ?
H6A O6 H6B 102(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re01 C1 1.882(7) y
Re01 C3 1.897(6) y
Re01 C2 1.899(7) y
Re01 O4 2.123(5) y
Re01 O5 2.146(4) y
Re01 O6 2.170(5) y
Br1 C12 1.899(6) ?
O4 C17 1.278(7) ?
C11 O5 1.289(7) ?
C11 C12 1.408(9) ?
C11 C17 1.477(8) ?
C2 O2 1.171(8) ?
C15 C16 1.379(9) ?
C15 C14 1.398(9) ?
C15 H15 0.93 ?
C3 O3 1.162(8) ?
C17 C16 1.415(8) ?
C16 Br3 1.895(6) ?
C12 C13 1.372(9) ?
C13 C14 1.378(9) ?
C13 H13 0.93 ?
C14 Br2 1.900(6) ?
O1 C1 1.168(8) ?
O7 C4 1.495(8) ?
O7 H7 0.82 ?
C4 H4C 0.96 ?
C4 H4A 0.96 ?
C4 H4B 0.96 ?
O6 H6A 0.99(8) ?
O6 H6B 1.06(8) ?
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
O6 H6B Br1 2_666 1.06(8) 2.68(8) 3.421(6) 127(5)
O6 H6B O5 2_666 1.06(8) 1.86(8) 2.825(7) 149(6)
C15 H15 O2 1_445 0.93 2.5 3.409(8) 166
O7 H7 O1 2_667 0.82 2.39 2.986(7) 130
O6 H6A O7 . 0.99(8) 1.69(8) 2.665(7) 167(7)
