#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/04/4080436.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_4080436
loop_
_publ_author_name
'Zhao, Helen C.'
'Mello, Barbara'
'Fu, Bi-Li'
'Chowdhury, Hara'
'Szalda, David J.'
'Tsai, Ming-Kang'
'Grills, David C.'
'Rochford, Jonathan'
_publ_section_title
;
 Investigation of Monomeric versus Dimericfac-Rhenium(I) Tricarbonyl
 Systems Containing the Noninnocent 8-Oxyquinolate Ligand
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1832
_journal_paper_doi               10.1021/om301250v
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '(C28 H20 N2 O8 Re2) (H4 C3.5)'
_chemical_formula_sum            'C31.5 H24 N2 O8 Re2'
_chemical_formula_weight         930.93
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 110.476(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2393(10)
_cell_length_b                   9.0765(4)
_cell_length_c                   20.7384(10)
_cell_measurement_reflns_used    3394
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.48
_cell_volume                     3040.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16597
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.010
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
      SADABS Version 2007/2 (Sheldrick, Bruker AXS Inc.) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0501
_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)+(0.0360P)²+3.0995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                4389
_reflns_number_total             6870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301250v_si_002.cif
_cod_data_source_block           jrhc0120
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C31.50 H24 N2 O8 Re2'
_cod_database_code               4080436
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_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 0.23089(2) 0.17039(4) 0.072049(17) 0.03240(11) Uani 1 1 d .
O1 O 0.2073(5) 0.0502(9) -0.0715(3) 0.071(2) Uani 1 1 d .
C1 C 0.2170(6) 0.0937(12) -0.0164(6) 0.048(3) Uani 1 1 d .
O2 O 0.3637(5) 0.3740(9) 0.0565(4) 0.074(3) Uani 1 1 d .
C2 C 0.3154(7) 0.2990(12) 0.0627(5) 0.047(3) Uani 1 1 d .
O3 O 0.1162(5) 0.4112(9) -0.0112(4) 0.069(2) Uani 1 1 d .
C3 C 0.1564(7) 0.3201(11) 0.0216(5) 0.047(3) Uani 1 1 d .
N11 N 0.2528(5) 0.2341(8) 0.1791(3) 0.0302(17) Uani 1 1 d .
C12 C 0.2133(6) 0.3406(10) 0.1996(5) 0.038(2) Uani 1 1 d .
H12 H 0.1715 0.3933 0.1671 0.045 Uiso 1 1 calc R
C13 C 0.2345(7) 0.3741(11) 0.2704(5) 0.047(3) Uani 1 1 d .
H13 H 0.2042 0.4436 0.2845 0.056 Uiso 1 1 calc R
C14 C 0.2991(7) 0.3042(10) 0.3173(5) 0.045(3) Uani 1 1 d .
H14 H 0.3141 0.3282 0.3637 0.054 Uiso 1 1 calc R
C15 C 0.3442(6) 0.1954(10) 0.2968(4) 0.037(2) Uani 1 1 d .
C16 C 0.3169(5) 0.1614(9) 0.2262(4) 0.030(2) Uani 1 1 d .
C17 C 0.3526(5) 0.0454(10) 0.2007(4) 0.029(2) Uani 1 1 d .
O17 O 0.3129(3) 0.0045(6) 0.1344(3) 0.0292(14) Uani 1 1 d .
C18 C 0.4225(6) -0.0241(10) 0.2435(5) 0.036(2) Uani 1 1 d .
C181 C 0.4687(6) -0.1367(11) 0.2197(5) 0.051(3) Uani 1 1 d .
H18A H 0.4401 -0.1564 0.1718 0.076 Uiso 1 1 calc R
H18B H 0.4725 -0.2257 0.2457 0.076 Uiso 1 1 calc R
H18C H 0.5233 -0.1009 0.2263 0.076 Uiso 1 1 calc R
C19 C 0.4507(6) 0.0142(10) 0.3146(5) 0.043(2) Uani 1 1 d .
H19 H 0.4975 -0.0335 0.3439 0.051 Uiso 1 1 calc R
C20 C 0.4138(6) 0.1157(11) 0.3424(5) 0.043(3) Uani 1 1 d .
C201 C 0.4431(8) 0.1427(13) 0.4191(5) 0.072(4) Uani 1 1 d .
H20A H 0.4918 0.0849 0.4415 0.108 Uiso 1 1 calc R
H20B H 0.4003 0.1151 0.4364 0.108 Uiso 1 1 calc R
H20C H 0.4559 0.2453 0.4282 0.108 Uiso 1 1 calc R
Re2 Re 0.22571(2) -0.18357(4) 0.121285(17) 0.02871(11) Uani 1 1 d .
O4 O 0.2383(6) -0.2831(9) -0.0154(4) 0.082(3) Uani 1 1 d .
C4 C 0.2332(6) -0.2405(11) 0.0342(5) 0.040(2) Uani 1 1 d .
O5 O 0.3452(5) -0.4355(8) 0.1852(4) 0.066(2) Uani 1 1 d .
C5 C 0.3007(6) -0.3392(11) 0.1594(5) 0.036(2) Uani 1 1 d .
O6 O 0.0845(4) -0.4024(8) 0.0975(4) 0.0522(19) Uani 1 1 d .
C6 C 0.1380(6) -0.3214(10) 0.1060(4) 0.033(2) Uani 1 1 d .
N21 N 0.2095(5) -0.1125(8) 0.2156(3) 0.0327(18) Uani 1 1 d .
C22 C 0.2475(6) -0.1601(10) 0.2788(4) 0.039(2) Uani 1 1 d .
H22 H 0.2911 -0.2260 0.2864 0.047 Uiso 1 1 calc R
C23 C 0.2265(7) -0.1180(13) 0.3346(5) 0.055(3) Uani 1 1 d .
H23 H 0.2566 -0.1518 0.3786 0.066 Uiso 1 1 calc R
C24 C 0.1605(7) -0.0254(12) 0.3236(5) 0.054(3) Uani 1 1 d .
H24 H 0.1442 0.0000 0.3604 0.065 Uiso 1 1 calc R
C25 C 0.1171(6) 0.0317(11) 0.2587(5) 0.040(2) Uani 1 1 d .
C26 C 0.1446(5) -0.0139(9) 0.2041(4) 0.0260(19) Uani 1 1 d .
O27 O 0.1458(4) 0.0072(6) 0.0911(3) 0.0281(14) Uani 1 1 d .
C27 C 0.1079(6) 0.0422(10) 0.1374(4) 0.031(2) Uani 1 1 d .
C28 C 0.0387(6) 0.1278(11) 0.1209(5) 0.041(2) Uani 1 1 d .
C28A C -0.0072(6) 0.1836(11) 0.0498(5) 0.051(3) Uani 1 1 d .
H28A H 0.0211 0.1537 0.0195 0.076 Uiso 1 1 calc R
H28B H -0.0101 0.2892 0.0506 0.076 Uiso 1 1 calc R
H28C H -0.0623 0.1436 0.0337 0.076 Uiso 1 1 calc R
C29 C 0.0098(7) 0.1650(12) 0.1755(6) 0.056(3) Uani 1 1 d .
H29 H -0.0378 0.2225 0.1645 0.067 Uiso 1 1 calc R
C230 C 0.0460(8) 0.1233(13) 0.2418(6) 0.060(3) Uani 1 1 d .
C231 C 0.0135(10) 0.1727(17) 0.2984(7) 0.109(6) Uani 1 1 d .
H31A H 0.0523 0.2396 0.3290 0.164 Uiso 1 1 calc R
H31B H 0.0068 0.0882 0.3239 0.164 Uiso 1 1 calc R
H31C H -0.0389 0.2211 0.2779 0.164 Uiso 1 1 calc R
C1T C 0.4435(15) 0.004(3) 0.0308(15) 0.112(8) Uani 1 1 d .
C2T C 0.519(2) 0.079(3) 0.0635(17) 0.164(11) Uani 1 1 d .
C3T C 0.4188(18) -0.071(4) -0.031(2) 0.190(16) Uani 1 1 d .
C4T C 0.552(3) 0.147(5) 0.108(2) 0.15(2) Uani 0.50 1 d P
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Re1 C3 84.1(4) . . y
C1 Re1 C2 88.2(4) . . y
C3 Re1 C2 84.3(5) . . y
C1 Re1 O17 99.1(3) . . y
C3 Re1 O17 176.5(3) . . y
C2 Re1 O17 97.1(4) . . y
C1 Re1 N11 173.4(4) . . y
C3 Re1 N11 102.2(4) . . y
C2 Re1 N11 94.2(3) . . y
O17 Re1 N11 74.5(2) . . y
C1 Re1 O27 93.4(3) . . y
C3 Re1 O27 102.3(4) . . y
C2 Re1 O27 173.3(4) . . y
O17 Re1 O27 76.2(2) . . y
N11 Re1 O27 83.4(2) . . y
O1 C1 Re1 178.1(10) . . y
O2 C2 Re1 179.2(11) . . y
O3 C3 Re1 174.7(10) . . y
C12 N11 C16 119.9(7) . . ?
C12 N11 Re1 125.9(6) . . ?
C16 N11 Re1 114.1(6) . . ?
N11 C12 C13 120.7(8) . . ?
N11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 119.6(9) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.8(9) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 116.7(9) . . ?
C16 C15 C20 118.2(9) . . ?
C14 C15 C20 125.1(9) . . ?
N11 C16 C15 122.2(8) . . ?
N11 C16 C17 116.3(7) . . ?
C15 C16 C17 121.5(8) . . ?
O17 C17 C18 123.2(8) . . ?
O17 C17 C16 116.9(8) . . ?
C18 C17 C16 119.9(8) . . ?
C17 O17 Re1 114.2(5) . . ?
C17 O17 Re2 114.4(5) . . ?
Re1 O17 Re2 100.9(2) . . y
C17 C18 C19 117.5(8) . . ?
C17 C18 C181 123.6(8) . . ?
C19 C18 C181 119.0(8) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C20 C19 C18 124.3(9) . . ?
C20 C19 H19 117.9 . . ?
C18 C19 H19 117.9 . . ?
C19 C20 C15 118.1(8) . . ?
C19 C20 C201 121.5(10) . . ?
C15 C20 C201 120.4(10) . . ?
C20 C201 H20A 109.5 . . ?
C20 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
C20 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
C5 Re2 C6 88.0(4) . . y
C5 Re2 C4 86.1(4) . . y
C6 Re2 C4 88.7(4) . . y
C5 Re2 O27 172.4(3) . . y
C6 Re2 O27 95.1(3) . . y
C4 Re2 O27 100.9(3) . . y
C5 Re2 N21 97.5(3) . . y
C6 Re2 N21 90.0(3) . . y
C4 Re2 N21 176.2(3) . . y
O27 Re2 N21 75.7(2) . . y
C5 Re2 O17 100.9(3) . . y
C6 Re2 O17 171.0(3) . . y
C4 Re2 O17 93.3(3) . . y
O27 Re2 O17 75.9(2) . . y
N21 Re2 O17 87.5(2) . . y
O4 C4 Re2 175.5(10) . . y
O5 C5 Re2 176.9(9) . . y
O6 C6 Re2 178.5(8) . . y
C22 N21 C26 118.2(7) . . ?
C22 N21 Re2 128.7(6) . . ?
C26 N21 Re2 112.9(5) . . ?
N21 C22 C23 124.0(9) . . ?
N21 C22 H22 118.0 . . ?
C23 C22 H22 118.0 . . ?
C24 C23 C22 118.5(9) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C23 C24 C25 121.6(9) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C230 125.6(9) . . ?
C24 C25 C26 116.2(9) . . ?
C230 C25 C26 118.1(9) . . ?
N21 C26 C27 117.6(7) . . ?
N21 C26 C25 121.5(8) . . ?
C27 C26 C25 120.9(8) . . ?
C27 O27 Re2 113.2(5) . . ?
C27 O27 Re1 118.5(5) . . ?
Re2 O27 Re1 101.1(2) . . ?
C28 C27 O27 122.9(8) . . ?
C28 C27 C26 120.7(8) . . ?
O27 C27 C26 116.4(8) . . ?
C27 C28 C29 116.9(9) . . ?
C27 C28 C28A 123.8(9) . . ?
C29 C28 C28A 119.3(9) . . ?
C28 C28A H28A 109.5 . . ?
C28 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C28 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C230 C29 C28 125.1(10) . . ?
C230 C29 H29 117.4 . . ?
C28 C29 H29 117.4 . . ?
C29 C230 C25 117.8(10) . . ?
C29 C230 C231 122.3(11) . . ?
C25 C230 C231 119.9(11) . . ?
C230 C231 H31A 109.5 . . ?
C230 C231 H31B 109.5 . . ?
H31A C231 H31B 109.5 . . ?
C230 C231 H31C 109.5 . . ?
H31A C231 H31C 109.5 . . ?
H31B C231 H31C 109.5 . . ?
C3T C1T C2T 128(2) . . ?
C4T C2T C1T 143(6) . . ?
C4T C2T C3T 99(5) . 3_655 ?
C1T C2T C3T 118(3) . 3_655 ?
C1T C3T C2T 115(3) . 3_655 ?
C1T C3T C4T 148(3) . 3_655 ?
C2T C3T C4T 33.6(19) 3_655 3_655 ?
C2T C4T C3T 47(3) . 3_655 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C1 1.897(12) . y
Re1 C3 1.911(10) . y
Re1 C2 1.930(11) . y
Re1 O17 2.158(5) . y
Re1 N11 2.195(7) . y
Re1 O27 2.216(5) . y
O1 C1 1.165(11) . y
O2 C2 1.117(11) . y
O3 C3 1.139(11) . y
N11 C12 1.335(11) . ?
N11 C16 1.362(10) . ?
C12 C13 1.415(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.354(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.411(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.406(11) . ?
C15 C20 1.437(13) . ?
C16 C17 1.413(11) . ?
C17 O17 1.357(9) . ?
C17 C18 1.374(12) . ?
O17 Re2 2.227(5) . y
C18 C19 1.424(12) . ?
C18 C181 1.482(12) . ?
C181 H18A 0.9600 . ?
C181 H18B 0.9600 . ?
C181 H18C 0.9600 . ?
C19 C20 1.357(13) . ?
C19 H19 0.9300 . ?
C20 C201 1.512(12) . ?
C201 H20A 0.9600 . ?
C201 H20B 0.9600 . ?
C201 H20C 0.9600 . ?
Re2 C5 1.891(10) . y
Re2 C6 1.901(10) . y
Re2 C4 1.925(10) . y
Re2 O27 2.165(5) . y
Re2 N21 2.168(6) . y
O4 C4 1.130(11) . y
O5 C5 1.163(10) . y
O6 C6 1.145(10) . y
N21 C22 1.318(10) . ?
N21 C26 1.386(11) . ?
C22 C23 1.380(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.369(14) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(13) . ?
C24 H24 0.9300 . ?
C25 C230 1.419(14) . ?
C25 C26 1.433(11) . ?
C26 C27 1.400(11) . ?
O27 C27 1.374(9) . ?
C27 C28 1.362(12) . ?
C28 C29 1.430(13) . ?
C28 C28A 1.497(12) . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C29 C230 1.351(14) . ?
C29 H29 0.9300 . ?
C230 C231 1.534(14) . ?
C231 H31A 0.9600 . ?
C231 H31B 0.9600 . ?
C231 H31C 0.9600 . ?
C1T C3T 1.39(4) . ?
C1T C2T 1.41(3) . ?
C2T C4T 1.09(4) . ?
C2T C3T 1.45(3) 3_655 ?
C3T C2T 1.45(3) 3_655 ?
C3T C4T 1.95(6) 3_655 ?
C4T C3T 1.95(6) 3_655 ?
