#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/70/7107095.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7107095
loop_
_publ_author_name
'Celedonio Alvarez'
'Romen Carrillo'
'Raul Garcia-Rodriguez'
'Daniel Miguel'
_publ_section_title
;
 pH-driven dynamic stereoinduction: epimerization upon dimerization in
 rhenium(I) complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              12765
_journal_paper_doi               10.1039/c1cc14799d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C22.5 H21 Cl F3 N2 O8 Re S'
_chemical_formula_weight         758.12
_chemical_name_systematic
;
?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.330(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.040(13)
_cell_length_b                   19.262(12)
_cell_length_c                   14.903(9)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.698
_cell_measurement_theta_min      2.897
_cell_volume                     5699(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
M. C. Burla, M. Camalli, B. Carrozzini, G. L. Cascarano, C. Giacovazzo,
G. Polidori and R. Spagna. J. Appl. Cryst. (2003). 36, 1103.'
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27620
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    4.497
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.454460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.132
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0341
_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/[σ²(Fo²)+(0.0413P)²+7.7553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                4509
_reflns_number_total             6995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14799d.txt
_cod_data_source_block           Compound_7b_rg555cm
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C22.50 H21 Cl F3 N2 O8 Re S'
_cod_database_code               7107095
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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.114609(9) 0.123708(11) 0.165831(14) 0.04839(8) Uani 1 1 d .
N1 N 0.2214(2) 0.0984(2) 0.2014(3) 0.0468(10) Uani 1 1 d .
C1 C 0.0237(3) 0.1578(3) 0.1239(5) 0.0666(16) Uani 1 1 d .
O1 O -0.0298(2) 0.1788(3) 0.1000(4) 0.1033(17) Uani 1 1 d .
C2 C 0.0951(3) 0.0733(3) 0.2635(5) 0.0623(14) Uani 1 1 d .
O2 O 0.0848(2) 0.0422(2) 0.3229(3) 0.0879(14) Uani 1 1 d .
C3 C 0.0893(3) 0.0410(3) 0.0844(4) 0.0615(14) Uani 1 1 d .
O3 O 0.0751(2) -0.0093(2) 0.0419(4) 0.0945(15) Uani 1 1 d .
H4 H 0.141(3) 0.229(3) 0.049(4) 0.081(19) Uiso 1 1 d .
O4 O 0.14831(17) 0.17772(19) 0.0605(2) 0.0532(9) Uani 1 1 d .
O5 O 0.1778(2) 0.2146(2) -0.1300(3) 0.0842(13) Uani 1 1 d .
C11 C 0.2582(3) 0.0642(3) 0.2812(4) 0.0616(15) Uani 1 1 d .
H11 H 0.2366 0.0484 0.3226 0.074 Uiso 1 1 calc R
C12 C 0.3251(3) 0.0522(3) 0.3031(4) 0.0726(17) Uani 1 1 d .
H12 H 0.3485 0.0283 0.3583 0.087 Uiso 1 1 calc R
C13 C 0.3577(3) 0.0754(4) 0.2441(5) 0.0786(19) Uani 1 1 d .
H13 H 0.4034 0.0668 0.2576 0.094 Uiso 1 1 calc R
C14 C 0.3217(3) 0.1117(3) 0.1638(4) 0.0682(16) Uani 1 1 d .
H14 H 0.3433 0.1293 0.1234 0.082 Uiso 1 1 calc R
C15 C 0.2538(2) 0.1219(2) 0.1436(3) 0.0464(11) Uani 1 1 d .
C16 C 0.2130(3) 0.1585(3) 0.0536(3) 0.0497(12) Uani 1 1 d .
H16 H 0.2368 0.2010 0.0474 0.060 Uiso 1 1 calc R
C17 C 0.2034(3) 0.1143(3) -0.0337(4) 0.0558(13) Uani 1 1 d .
H17A H 0.2447 0.0886 -0.0250 0.067 Uiso 1 1 calc R
H17B H 0.1682 0.0807 -0.0381 0.067 Uiso 1 1 calc R
C18 C 0.1858(3) 0.1522(3) -0.1255(4) 0.0628(15) Uani 1 1 d .
C19 C 0.1784(5) 0.1112(4) -0.2129(5) 0.095(2) Uani 1 1 d .
H19A H 0.1543 0.1380 -0.2678 0.143 Uiso 1 1 calc R
H19B H 0.1539 0.0693 -0.2118 0.143 Uiso 1 1 calc R
H19C H 0.2221 0.0997 -0.2154 0.143 Uiso 1 1 calc R
C31 C 0.1481(3) 0.2086(3) 0.2559(4) 0.0516(12) Uani 1 1 d .
N31 N 0.1693(2) 0.2535(2) 0.3080(3) 0.0533(10) Uani 1 1 d .
C32 C 0.2009(3) 0.3087(3) 0.3676(3) 0.0521(13) Uani 1 1 d .
C33 C 0.1617(3) 0.3625(3) 0.3837(4) 0.0597(15) Uani 1 1 d .
C34 C 0.1971(4) 0.4163(3) 0.4418(5) 0.081(2) Uani 1 1 d .
H34 H 0.1735 0.4535 0.4551 0.098 Uiso 1 1 calc R
C35 C 0.2655(4) 0.4152(4) 0.4792(5) 0.084(2) Uani 1 1 d .
H35 H 0.2879 0.4526 0.5155 0.101 Uiso 1 1 calc R
C36 C 0.3016(4) 0.3606(3) 0.4645(4) 0.0763(19) Uani 1 1 d .
H36 H 0.3481 0.3605 0.4935 0.092 Uiso 1 1 calc R
C37 C 0.2711(3) 0.3052(3) 0.4074(4) 0.0595(15) Uani 1 1 d .
C38 C 0.0875(4) 0.3590(4) 0.3437(6) 0.100(3) Uani 1 1 d .
H38A H 0.0741 0.3539 0.2759 0.150 Uiso 1 1 calc R
H38B H 0.0685 0.4008 0.3588 0.150 Uiso 1 1 calc R
H38C H 0.0717 0.3199 0.3703 0.150 Uiso 1 1 calc R
C39 C 0.3105(3) 0.2451(3) 0.3897(5) 0.0816(19) Uani 1 1 d .
H39A H 0.2915 0.2025 0.4025 0.122 Uiso 1 1 calc R
H39B H 0.3565 0.2486 0.4305 0.122 Uiso 1 1 calc R
H39C H 0.3088 0.2456 0.3245 0.122 Uiso 1 1 calc R
C51 C 0.0223(5) 0.3714(6) -0.0422(9) 0.120(3) Uani 1 1 d .
F51 F -0.0142(4) 0.4180(5) -0.0264(6) 0.206(4) Uani 1 1 d .
F52 F 0.0281(4) 0.3730(5) -0.1244(5) 0.222(5) Uani 1 1 d .
F53 F -0.0094(4) 0.3144(6) -0.0335(8) 0.268(5) Uani 1 1 d .
S51 S 0.10527(10) 0.36786(10) 0.04971(13) 0.0835(5) Uani 1 1 d .
O51 O 0.1356(3) 0.3094(2) 0.0206(5) 0.126(2) Uani 1 1 d .
O52 O 0.0912(5) 0.3625(6) 0.1309(6) 0.239(6) Uani 1 1 d .
O53 O 0.1361(3) 0.4319(3) 0.0301(5) 0.1190(19) Uani 1 1 d .
C90 C 0.0000 0.2011(9) 0.7500 0.174(7) Uani 1 2 d S
H90A H -0.0396 0.2304 0.7351 0.208 Uiso 0.50 1 calc PR
H90B H 0.0396 0.2304 0.7649 0.208 Uiso 0.50 1 calc PR
Cl1 Cl 0.0049(2) 0.1446(3) 0.8468(3) 0.230(2) Uani 1 1 d .
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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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_site_symmetry_1
C2 Re1 C1 88.8(3) .
C2 Re1 C3 88.6(2) .
C1 Re1 C3 92.3(2) .
C2 Re1 C31 91.1(2) .
C1 Re1 C31 91.7(2) .
C3 Re1 C31 176.1(2) .
C2 Re1 N1 99.5(2) .
C1 Re1 N1 171.2(2) .
C3 Re1 N1 90.9(2) .
C31 Re1 N1 85.29(18) .
C2 Re1 O4 173.77(19) .
C1 Re1 O4 97.4(2) .
C3 Re1 O4 91.6(2) .
C31 Re1 O4 88.20(18) .
N1 Re1 O4 74.25(14) .
C15 N1 C11 117.6(5) .
C15 N1 Re1 118.0(3) .
C11 N1 Re1 124.3(4) .
O1 C1 Re1 179.0(6) .
O2 C2 Re1 178.4(5) .
O3 C3 Re1 175.9(6) .
C16 O4 Re1 117.7(3) .
C12 C11 N1 122.6(6) .
C11 C12 C13 119.7(6) .
C12 C13 C14 118.7(6) .
C15 C14 C13 119.7(6) .
N1 C15 C14 121.6(5) .
N1 C15 C16 117.9(4) .
C14 C15 C16 120.5(5) .
O4 C16 C15 109.2(4) .
O4 C16 C17 110.3(4) .
C15 C16 C17 112.2(4) .
C18 C17 C16 116.0(5) .
O5 C18 C17 121.7(6) .
O5 C18 C19 120.4(6) .
C17 C18 C19 117.9(5) .
N31 C31 Re1 176.7(5) .
C31 N31 C32 173.9(5) .
C33 C32 C37 124.4(5) .
C33 C32 N31 119.3(5) .
C37 C32 N31 116.4(5) .
C32 C33 C34 115.7(6) .
C32 C33 C38 120.2(6) .
C34 C33 C38 124.0(6) .
C35 C34 C33 121.1(6) .
C36 C35 C34 121.3(6) .
C35 C36 C37 121.8(6) .
C36 C37 C32 115.7(6) .
C36 C37 C39 122.3(6) .
C32 C37 C39 122.0(5) .
F51 C51 F52 115.1(11) .
F51 C51 F53 102.6(9) .
F52 C51 F53 109.3(12) .
F51 C51 S51 112.2(10) .
F52 C51 S51 110.5(7) .
F53 C51 S51 106.5(9) .
O52 S51 O51 117.8(5) .
O52 S51 O53 119.2(6) .
O51 S51 O53 109.3(4) .
O52 S51 C51 103.8(6) .
O51 S51 C51 102.3(5) .
O53 S51 C51 101.2(4) .
Cl1 C90 Cl1 104.8(9) 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C2 1.905(7) .
Re1 C1 1.921(6) .
Re1 C3 1.967(6) .
Re1 C31 2.084(6) .
Re1 N1 2.186(4) .
Re1 O4 2.187(4) .
N1 C15 1.341(6) .
N1 C11 1.356(6) .
C1 O1 1.137(7) .
C2 O2 1.148(7) .
C3 O3 1.141(6) .
O4 C16 1.447(6) .
O5 C18 1.214(7) .
C11 C12 1.355(8) .
C12 C13 1.357(9) .
C13 C14 1.376(8) .
C14 C15 1.373(8) .
C15 C16 1.507(7) .
C16 C17 1.511(7) .
C17 C18 1.485(8) .
C18 C19 1.486(9) .
C31 N31 1.150(6) .
N31 C32 1.403(6) .
C32 C33 1.394(8) .
C32 C37 1.399(8) .
C33 C34 1.398(9) .
C33 C38 1.477(10) .
C34 C35 1.359(10) .
C35 C36 1.357(10) .
C36 C37 1.384(8) .
C37 C39 1.498(8) .
C51 F51 1.253(12) .
C51 F52 1.271(12) .
C51 F53 1.313(12) .
C51 S51 1.829(11) .
S51 O52 1.342(7) .
S51 O51 1.430(5) .
S51 O53 1.468(6) .
C90 Cl1 1.783(10) 2_556
C90 Cl1 1.783(10) .
