#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/06/7020673.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_7020673
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            'C22 H31 F8.38 N10 O4.42 P1.4 Re1.61'
_chemical_formula_weight         1007.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.1330(10)
_cell_angle_beta                 97.5260(10)
_cell_angle_gamma                101.0040(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3330(5)
_cell_length_b                   9.7967(6)
_cell_length_c                   11.5140(7)
_cell_measurement_reflns_used    6192
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.33
_cell_volume                     833.14(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10815
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    5.996
_exptl_absorpt_correction_T_max  0.3193
_exptl_absorpt_correction_T_min  0.1193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             484.8
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3821
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²+2.0377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                3672
_reflns_number_total             3821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31681a.txt
_cod_data_source_block           a616
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        833.13(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C22 H31 F8.38 N10 O4.42 P1.40 Re1.61'
_cod_database_code               7020673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Re1 Re 0.5000 0.5000 0.0000 0.04350(12) Uani 1 2 d SU . .
O1 O 0.7207(5) 0.5757(4) -0.0246(3) 0.0395(6) Uani 1 1 d DU . .
H1O H 0.698(14) 0.618(12) -0.074(9) 0.047 Uiso 0.50 1 d PD . .
N1 N 0.7423(5) 0.3570(5) 0.1368(4) 0.0401(9) Uani 1 1 d . . .
N2 N 0.5991(5) 0.4776(4) 0.2601(4) 0.0331(8) Uani 1 1 d . . .
N3 N 0.5296(5) 0.7094(4) 0.2857(4) 0.0341(8) Uani 1 1 d . . .
N4 N 0.5960(5) 0.8566(4) 0.1928(4) 0.0368(9) Uani 1 1 d . . .
C1 C 0.6230(6) 0.4328(5) 0.1384(4) 0.0326(9) Uani 1 1 d . . .
C2 C 0.7932(7) 0.3568(6) 0.2555(5) 0.0455(12) Uani 1 1 d . . .
H2B H 0.8758 0.3123 0.2779 0.055 Uiso 1 1 calc R . .
C3 C 0.7031(7) 0.4318(6) 0.3333(5) 0.0418(11) Uani 1 1 d . . .
H3B H 0.7095 0.4496 0.4201 0.050 Uiso 1 1 calc R . .
C4 C 0.4860(6) 0.5715(6) 0.3077(4) 0.0365(10) Uani 1 1 d . . .
H4B H 0.3699 0.5145 0.2628 0.044 Uiso 1 1 calc R . .
H4C H 0.4956 0.5985 0.3998 0.044 Uiso 1 1 calc R . .
C5 C 0.5414(6) 0.7081(5) 0.1695(4) 0.0309(9) Uani 1 1 d . . .
C6 C 0.5765(7) 0.8568(6) 0.3803(5) 0.0437(12) Uani 1 1 d . . .
H6A H 0.5786 0.8867 0.4683 0.052 Uiso 1 1 calc R . .
C7 C 0.6184(7) 0.9487(6) 0.3209(5) 0.0461(12) Uani 1 1 d . . .
H7A H 0.6559 1.0559 0.3598 0.055 Uiso 1 1 calc R . .
C8 C 0.8191(8) 0.2915(8) 0.0276(6) 0.0581(16) Uani 1 1 d . . .
H8A H 0.7642 0.3037 -0.0461 0.087 Uiso 1 1 calc R . .
H8B H 0.8063 0.1838 0.0065 0.087 Uiso 1 1 calc R . .
H8C H 0.9373 0.3438 0.0505 0.087 Uiso 1 1 calc R . .
C9 C 0.6344(8) 0.9162(6) 0.0980(5) 0.0491(13) Uani 1 1 d . . .
H9A H 0.6096 0.8323 0.0138 0.074 Uiso 1 1 calc R . .
H9B H 0.7523 0.9699 0.1214 0.074 Uiso 1 1 calc R . .
H9C H 0.5668 0.9859 0.0960 0.074 Uiso 1 1 calc R . .
P1 P 0.7852(9) 0.8499(7) 0.7320(7) 0.0423(3) Uani 0.6975(14) 1 d PD A 1
F1 F 0.6516(10) 0.7213(8) 0.6170(6) 0.129(5) Uani 0.6975(14) 1 d PD A 1
F2 F 0.9196(9) 0.8321(10) 0.6482(8) 0.170(6) Uani 0.6975(14) 1 d PD A 1
F3 F 0.9227(7) 0.9768(8) 0.8489(6) 0.125(3) Uani 0.6975(14) 1 d PD A 1
F4 F 0.6550(8) 0.8651(9) 0.8181(6) 0.096(2) Uani 0.6975(14) 1 d PD A 1
F5 F 0.7392(8) 0.9719(7) 0.6903(7) 0.092(2) Uani 0.6975(14) 1 d PD A 1
F6 F 0.8356(10) 0.7251(9) 0.7748(9) 0.121(4) Uani 0.6975(14) 1 d PD A 1
Re2 Re 0.7907(3) 0.8273(2) 0.7362(2) 0.0423(3) Uani 0.3025(14) 1 d PD A 2
O2 O 0.817(2) 0.746(2) 0.8426(15) 0.115(12) Uani 0.3025(14) 1 d PD A 2
O3 O 0.9716(18) 0.8747(19) 0.6990(19) 0.097(10) Uani 0.3025(14) 1 d PD A 2
O4 O 0.714(2) 0.9747(18) 0.7983(19) 0.138(13) Uani 0.3025(14) 1 d PD A 2
O5 O 0.6508(19) 0.6916(18) 0.6022(14) 0.051(5) Uani 0.3025(14) 1 d PD A 2
C1S C -0.0259(11) 0.7742(13) 0.3238(14) 0.130(5) Uani 1 1 d . . .
H1S1 H -0.1345 0.7149 0.3218 0.196 Uiso 1 1 calc R . .
H1S2 H -0.0159 0.7569 0.2367 0.196 Uiso 1 1 calc R . .
H1S3 H -0.0151 0.8818 0.3731 0.196 Uiso 1 1 calc R . .
C2S C 0.1045(8) 0.7280(8) 0.3829(7) 0.0605(16) Uani 1 1 d . . .
N1S N 0.2056(8) 0.6956(8) 0.4315(7) 0.0806(18) 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'
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
O1 Re1 O1 180.0(2) 2_665 .
O1 Re1 C5 90.60(15) 2_665 .
O1 Re1 C5 89.40(15) . .
O1 Re1 C5 89.40(15) 2_665 2_665
O1 Re1 C5 90.60(15) . 2_665
C5 Re1 C5 180.000(1) . 2_665
O1 Re1 C1 92.30(15) 2_665 .
O1 Re1 C1 87.70(15) . .
C5 Re1 C1 81.42(16) . .
C5 Re1 C1 98.58(16) 2_665 .
O1 Re1 C1 87.70(15) 2_665 2_665
O1 Re1 C1 92.30(15) . 2_665
C5 Re1 C1 98.58(16) . 2_665
C5 Re1 C1 81.42(16) 2_665 2_665
C1 Re1 C1 180.0 . 2_665
C1 N1 C2 110.9(4) . .
C1 N1 C8 125.7(4) . .
C2 N1 C8 123.2(5) . .
C1 N2 C3 111.4(4) . .
C1 N2 C4 123.3(4) . .
C3 N2 C4 125.2(4) . .
C5 N3 C6 111.2(4) . .
C5 N3 C4 123.3(4) . .
C6 N3 C4 125.3(4) . .
C5 N4 C7 111.2(4) . .
C5 N4 C9 125.9(4) . .
C7 N4 C9 122.8(4) . .
N1 C1 N2 104.2(4) . .
N1 C1 Re1 133.1(3) . .
N2 C1 Re1 122.4(3) . .
C3 C2 N1 107.4(4) . .
C2 C3 N2 106.1(5) . .
N3 C4 N2 109.1(4) . .
N4 C5 N3 104.3(4) . .
N4 C5 Re1 132.7(3) . .
N3 C5 Re1 122.7(3) . .
C7 C6 N3 106.2(4) . .
C6 C7 N4 107.0(4) . .
F5 P1 F1 91.2(4) . .
F5 P1 F4 91.5(5) . .
F1 P1 F4 90.5(4) . .
F5 P1 F2 90.4(4) . .
F1 P1 F2 90.2(4) . .
F4 P1 F2 178.0(6) . .
F5 P1 F3 90.3(4) . .
F1 P1 F3 178.5(5) . .
F4 P1 F3 89.9(4) . .
F2 P1 F3 89.3(4) . .
F5 P1 F6 179.1(5) . .
F1 P1 F6 89.3(4) . .
F4 P1 F6 89.3(6) . .
F2 P1 F6 88.8(4) . .
F3 P1 F6 89.2(5) . .
O4 Re2 O3 112.3(6) . .
O4 Re2 O5 109.7(6) . .
O3 Re2 O5 109.4(6) . .
O4 Re2 O2 109.6(6) . .
O3 Re2 O2 109.2(6) . .
O5 Re2 O2 106.6(6) . .
N1S C2S C1S 178.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O1 1.946(4) 2_665
Re1 O1 1.946(4) .
Re1 C5 2.154(4) .
Re1 C5 2.154(4) 2_665
Re1 C1 2.155(5) .
Re1 C1 2.155(5) 2_665
N1 C1 1.348(6) .
N1 C2 1.378(7) .
N1 C8 1.470(7) .
N2 C1 1.356(6) .
N2 C3 1.380(6) .
N2 C4 1.456(6) .
N3 C5 1.350(6) .
N3 C6 1.382(6) .
N3 C4 1.454(6) .
N4 C5 1.348(6) .
N4 C7 1.373(6) .
N4 C9 1.461(7) .
C2 C3 1.340(8) .
C6 C7 1.344(8) .
P1 F5 1.538(6) .
P1 F1 1.549(7) .
P1 F4 1.553(7) .
P1 F2 1.564(7) .
P1 F3 1.569(7) .
P1 F6 1.584(6) .
Re2 O4 1.643(12) .
Re2 O3 1.650(14) .
Re2 O5 1.703(13) .
Re2 O2 1.706(14) .
C1S C2S 1.440(11) .
C2S N1S 1.112(9) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O2 0.840(10) 2.04(8) 2.741(14) 140(10) 1_554
O1 H1O F6 0.840(10) 2.62(7) 3.314(8) 140(10) 1_554
