#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (Tue 16 de Feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/06/7020675.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_7020675
loop_
_publ_author_name
'Lum, Regina'
'Zhang, Hu'
'Zhang, Wenhua'
'Bai, Shi-Qiang'
'Zhao, Jin'
'Hor, T. S. Andy'
_publ_section_title
;
 Trans [O=Re(V)-OH] core stabilised by chelating N-heterocyclic dicarbene
 ligands.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              871
_journal_page_last               873
_journal_paper_doi               10.1039/c2dt31681a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C50 H53 F7.8 N12 O4.8 P1.3 Re1.7'
_chemical_formula_weight         1378.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.7910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6582(6)
_cell_length_b                   11.1157(6)
_cell_length_c                   22.0292(12)
_cell_measurement_reflns_used    2870
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      21.31
_cell_measurement_theta_min      2.20
_cell_volume                     2783.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19182
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_T_max  0.7280
_exptl_absorpt_correction_T_min  0.5805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1385.20
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0512P)²+5.4129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                4936
_reflns_number_total             6379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31681a.txt
_cod_data_source_block           a051
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C50 H53 F7.8 N12 O4.8 P1.30 Re1.70'
_cod_database_code               7020675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C3S C 0.4740(18) 0.8877(17) 0.8956(9) 0.222(9) Uani 1 1 d DU . .
H3S1 H 0.4788 0.9293 0.8575 0.333 Uiso 1 1 calc R . .
H3S2 H 0.4389 0.8091 0.8855 0.333 Uiso 1 1 calc R . .
H3S3 H 0.5524 0.8784 0.9215 0.333 Uiso 1 1 calc R . .
C4S C 0.4027(16) 0.9566(15) 0.9287(9) 0.152(6) Uani 1 1 d DU . .
N2S N 0.3465(12) 1.0086(12) 0.9564(9) 0.175(7) Uani 1 1 d DU . .
P1 P 0.8035(7) 0.4556(7) 0.1861(4) 0.062(3) Uani 0.6498(18) 1 d PDU A 1
F1 F 0.7598(7) 0.4915(8) 0.1145(3) 0.101(2) Uani 0.6498(18) 1 d PD A 1
F2 F 0.6768(6) 0.4760(8) 0.1966(5) 0.089(2) Uani 0.6498(18) 1 d PD A 1
F3 F 0.8516(8) 0.4350(9) 0.2576(3) 0.101(2) Uani 0.6498(18) 1 d PD A 1
F4 F 0.9341(5) 0.4500(7) 0.1758(4) 0.089(2) Uani 0.6498(18) 1 d PD A 1
F5 F 0.8279(8) 0.6001(7) 0.1980(5) 0.100(2) Uani 0.6498(18) 1 d PDU A 1
F6 F 0.7848(7) 0.3239(6) 0.1711(4) 0.100(2) Uani 0.6498(18) 1 d PD A 1
Re2 Re 0.80255(19) 0.4767(2) 0.18913(11) 0.0484(5) Uani 0.3502(18) 1 d PD A 2
O1R O 0.8155(19) 0.6291(9) 0.1989(11) 0.121(10) Uani 0.3502(18) 1 d PDU A 2
O2R O 0.9010(17) 0.399(2) 0.2435(12) 0.146(12) Uani 0.3502(18) 1 d PDU A 2
O3R O 0.6621(10) 0.4261(16) 0.1831(10) 0.089(8) Uani 0.3502(18) 1 d PDU A 2
O4R O 0.856(2) 0.438(2) 0.1249(9) 0.111(7) Uani 0.3502(18) 1 d PDU A 2
Re1 Re 0.0000 1.0000 0.0000 0.03627(13) Uani 1 2 d S . .
O1 O 0.1526(4) 1.0330(4) 0.0350(2) 0.0425(11) Uani 1 1 d D . .
H91 H 0.222(5) 1.062(14) 0.040(8) 0.07(6) Uiso 0.50 1 d PD . .
N1 N -0.0213(5) 1.0776(5) 0.1386(2) 0.0412(13) Uani 1 1 d . . .
N2 N -0.0978(5) 0.9077(5) 0.1112(2) 0.0428(13) Uani 1 1 d . . .
N3 N -0.0401(5) 0.7479(5) 0.0538(2) 0.0427(13) Uani 1 1 d . . .
N4 N 0.1106(5) 0.7311(5) 0.0129(2) 0.0424(13) Uani 1 1 d . . .
C1 C -0.0408(5) 1.0013(6) 0.0913(3) 0.0400(14) Uani 1 1 d U . .
C2 C -0.0667(7) 1.0365(8) 0.1871(3) 0.056(2) Uani 1 1 d U . .
H2A H -0.0633 1.0761 0.2251 0.067 Uiso 1 1 calc R . .
C3 C -0.1159(6) 0.9319(8) 0.1706(3) 0.0521(18) Uani 1 1 d U . .
H3A H -0.1554 0.8829 0.1942 0.062 Uiso 1 1 calc R . .
C4 C 0.0457(6) 1.1904(7) 0.1414(3) 0.0522(18) Uani 1 1 d U . .
H4A H -0.0022 1.2565 0.1517 0.063 Uiso 1 1 calc R . .
H4B H 0.0611 1.2068 0.1002 0.063 Uiso 1 1 calc R . .
C5 C 0.1615(4) 1.1875(5) 0.1887(2) 0.0476(17) Uani 1 1 d GU . .
C6 C 0.2472(5) 1.1032(5) 0.1841(2) 0.079(3) Uani 1 1 d GU . .
H6A H 0.2331 1.0463 0.1517 0.095 Uiso 1 1 calc R . .
C7 C 0.3539(4) 1.1029(6) 0.2274(3) 0.081(3) Uani 1 1 d GU . .
H7A H 0.4119 1.0459 0.2243 0.097 Uiso 1 1 calc R . .
C8 C 0.3748(4) 1.1869(6) 0.2754(3) 0.082(3) Uani 1 1 d GU . .
H8A H 0.4469 1.1867 0.3047 0.098 Uiso 1 1 calc R . .
C9 C 0.2891(6) 1.2712(6) 0.2799(3) 0.136(5) Uani 1 1 d GU . .
H9A H 0.3032 1.3280 0.3123 0.163 Uiso 1 1 calc R . .
C10 C 0.1824(5) 1.2715(5) 0.2366(3) 0.111(4) Uani 1 1 d GU . .
H10A H 0.1244 1.3285 0.2397 0.134 Uiso 1 1 calc R . .
C11 C -0.1364(6) 0.7993(7) 0.0752(3) 0.0485(17) Uani 1 1 d U . .
H11A H -0.1665 0.7409 0.1012 0.058 Uiso 1 1 calc R . .
H11B H -0.2001 0.8192 0.0395 0.058 Uiso 1 1 calc R . .
C12 C 0.0285(5) 0.8111(6) 0.0224(3) 0.0387(15) Uani 1 1 d U . .
C13 C -0.0017(7) 0.6308(7) 0.0613(3) 0.056(2) Uani 1 1 d U . .
H13A H -0.0355 0.5689 0.0807 0.068 Uiso 1 1 calc R . .
C14 C 0.0904(7) 0.6209(7) 0.0367(4) 0.058(2) Uani 1 1 d U . .
H14A H 0.1349 0.5507 0.0355 0.069 Uiso 1 1 calc R . .
C15 C 0.2100(6) 0.7560(7) -0.0159(3) 0.055(2) Uani 1 1 d U . .
H15A H 0.2037 0.8385 -0.0320 0.066 Uiso 1 1 calc R . .
H15B H 0.2068 0.7013 -0.0511 0.066 Uiso 1 1 calc R . .
C16 C 0.3256(6) 0.7410(7) 0.0296(4) 0.0516(18) Uani 1 1 d U . .
C17 C 0.4132(7) 0.6708(7) 0.0151(4) 0.064(2) Uani 1 1 d U . .
H17A H 0.3981 0.6287 -0.0229 0.077 Uiso 1 1 calc R . .
C18 C 0.5217(7) 0.6607(9) 0.0544(5) 0.082(3) Uani 1 1 d U . .
H18A H 0.5812 0.6145 0.0431 0.098 Uiso 1 1 calc R . .
C19 C 0.5421(8) 0.7196(9) 0.1112(5) 0.081(3) Uani 1 1 d U . .
H19A H 0.6151 0.7109 0.1393 0.097 Uiso 1 1 calc R . .
C20 C 0.4586(9) 0.7889(9) 0.1263(4) 0.086(3) Uani 1 1 d U . .
H20A H 0.4737 0.8308 0.1643 0.103 Uiso 1 1 calc R . .
C21 C 0.3497(8) 0.7986(9) 0.0855(4) 0.083(3) Uani 1 1 d U . .
H21A H 0.2911 0.8461 0.0968 0.100 Uiso 1 1 calc R . .
N1S N 0.2563(8) 0.3467(8) 0.0553(4) 0.099(3) Uani 1 1 d . . .
C1S C 0.3119(8) 0.3870(8) 0.0962(5) 0.075(3) Uani 1 1 d U . .
C2S C 0.3778(12) 0.4464(13) 0.1521(5) 0.129(5) Uani 1 1 d U . .
H2S1 H 0.3583 0.5313 0.1505 0.194 Uiso 1 1 calc R . .
H2S2 H 0.4614 0.4369 0.1546 0.194 Uiso 1 1 calc R . .
H2S3 H 0.3576 0.4105 0.1885 0.194 Uiso 1 1 calc R . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N2S C4S C3S 178(2) . .
F6 P1 F2 94.5(5) . .
F6 P1 F3 94.6(5) . .
F2 P1 F3 90.7(5) . .
F6 P1 F4 91.5(5) . .
F2 P1 F4 173.9(6) . .
F3 P1 F4 89.8(5) . .
F6 P1 F1 91.5(5) . .
F2 P1 F1 90.3(5) . .
F3 P1 F1 173.7(6) . .
F4 P1 F1 88.5(5) . .
F6 P1 F5 175.9(6) . .
F2 P1 F5 88.3(5) . .
F3 P1 F5 88.4(5) . .
F4 P1 F5 85.6(5) . .
F1 P1 F5 85.4(5) . .
O2R Re2 O3R 111.9(8) . .
O2R Re2 O1R 112.8(9) . .
O3R Re2 O1R 113.1(7) . .
O2R Re2 O4R 98.0(15) . .
O3R Re2 O4R 111.8(8) . .
O1R Re2 O4R 108.2(8) . .
O1 Re1 O1 180.000(1) . 3_575
O1 Re1 C12 89.3(2) . 3_575
O1 Re1 C12 90.7(2) 3_575 3_575
O1 Re1 C12 90.7(2) . .
O1 Re1 C12 89.3(2) 3_575 .
C12 Re1 C12 180.0(3) 3_575 .
O1 Re1 C1 90.0(2) . 3_575
O1 Re1 C1 90.0(2) 3_575 3_575
C12 Re1 C1 81.3(2) 3_575 3_575
C12 Re1 C1 98.7(2) . 3_575
O1 Re1 C1 90.0(2) . .
O1 Re1 C1 90.0(2) 3_575 .
C12 Re1 C1 98.7(2) 3_575 .
C12 Re1 C1 81.3(2) . .
C1 Re1 C1 180.000(1) 3_575 .
C1 N1 C2 111.8(6) . .
C1 N1 C4 125.1(6) . .
C2 N1 C4 123.0(6) . .
C1 N2 C3 110.0(6) . .
C1 N2 C11 124.8(6) . .
C3 N2 C11 125.2(6) . .
C12 N3 C13 109.7(6) . .
C12 N3 C11 123.6(6) . .
C13 N3 C11 126.6(6) . .
C12 N4 C14 109.9(6) . .
C12 N4 C15 126.5(6) . .
C14 N4 C15 123.5(6) . .
N1 C1 N2 104.3(6) . .
N1 C1 Re1 134.5(5) . .
N2 C1 Re1 121.3(5) . .
C3 C2 N1 107.5(6) . .
C2 C3 N2 106.4(7) . .
N1 C4 C5 113.3(6) . .
C6 C5 C10 120.0 . .
C6 C5 C4 120.7(4) . .
C10 C5 C4 119.3(4) . .
C7 C6 C5 120.0 . .
C6 C7 C8 120.0 . .
C9 C8 C7 120.0 . .
C8 C9 C10 120.0 . .
C9 C10 C5 120.0 . .
N3 C11 N2 109.8(5) . .
N4 C12 N3 104.7(6) . .
N4 C12 Re1 132.8(5) . .
N3 C12 Re1 122.5(4) . .
C14 C13 N3 107.7(7) . .
C13 C14 N4 107.9(7) . .
N4 C15 C16 111.6(6) . .
C21 C16 C17 117.5(7) . .
C21 C16 C15 121.8(7) . .
C17 C16 C15 120.7(7) . .
C18 C17 C16 121.8(8) . .
C17 C18 C19 118.8(8) . .
C20 C19 C18 120.4(8) . .
C19 C20 C21 119.6(9) . .
C16 C21 C20 121.7(8) . .
N1S C1S C2S 175.1(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3S C4S 1.441(15) .
C4S N2S 1.147(15) .
P1 F6 1.506(8) .
P1 F2 1.561(8) .
P1 F3 1.566(8) .
P1 F4 1.590(8) .
P1 F1 1.597(8) .
P1 F5 1.641(8) .
Re2 O2R 1.700(9) .
Re2 O3R 1.708(9) .
Re2 O1R 1.711(10) .
Re2 O4R 1.725(9) .
Re1 O1 1.813(4) .
Re1 O1 1.813(4) 3_575
Re1 C12 2.166(7) 3_575
Re1 C12 2.166(7) .
Re1 C1 2.166(7) 3_575
Re1 C1 2.166(7) .
N1 C1 1.325(8) .
N1 C2 1.371(9) .
N1 C4 1.471(9) .
N2 C1 1.359(8) .
N2 C3 1.397(8) .
N2 C11 1.458(9) .
N3 C12 1.362(8) .
N3 C13 1.375(9) .
N3 C11 1.430(9) .
N4 C12 1.356(8) .
N4 C14 1.373(9) .
N4 C15 1.466(9) .
C2 C3 1.311(11) .
C4 C5 1.512(7) .
C5 C6 1.3900 .
C5 C10 1.3900 .
C6 C7 1.3900 .
C7 C8 1.3900 .
C8 C9 1.3900 .
C9 C10 1.3900 .
C13 C14 1.311(11) .
C15 C16 1.500(9) .
C16 C21 1.360(11) .
C16 C17 1.378(10) .
C17 C18 1.370(11) .
C18 C19 1.385(13) .
C19 C20 1.341(13) .
C20 C21 1.387(11) .
N1S C1S 1.082(10) .
C1S C2S 1.458(13) .
