#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/99/7009975.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_7009975
loop_
_publ_author_name
'Burrell, Anthony K.'
'Steedman, Andrew J.'
_publ_section_title
;
 A systematic route to mixed imido complexes of rhenium
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2501
_journal_paper_doi               10.1039/b004938g
_journal_year                    2000
_chemical_formula_moiety         'C34 H47 Cl N3 Re'
_chemical_formula_sum            'C34 H47 Cl N3 Re'
_chemical_formula_weight         719.40
_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                80.3510(10)
_cell_angle_beta                 72.8540(10)
_cell_angle_gamma                81.98
_cell_formula_units_Z            2
_cell_length_a                   10.6026(2)
_cell_length_b                   10.6126(2)
_cell_length_c                   15.93340(10)
_cell_measurement_reflns_used    7245
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.35
_cell_volume                     1681.18(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'XPMA (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Siemens SMART 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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16481
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    3.718
_exptl_absorpt_correction_T_max  0.8077
_exptl_absorpt_correction_T_min  0.3323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.628
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.704
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.704
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                6755
_reflns_number_total             7301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004938g.txt
_cod_data_source_block           retbu
_cod_original_cell_volume        1681.19(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009975
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 0.918293(9) 0.638887(9) 0.716218(7) 0.02584(6) Uani 1 1 d . . .
Cl1 Cl 1.10591(9) 0.71208(9) 0.61483(6) 0.0459(2) Uani 1 1 d . . .
N1 N 0.9030(3) 0.6962(3) 0.81552(19) 0.0333(6) Uani 1 1 d . . .
C1A C 0.8751(3) 0.7345(3) 0.8987(2) 0.0331(6) Uani 1 1 d . . .
C2A C 0.7447(4) 0.7705(3) 0.9457(2) 0.0378(7) Uani 1 1 d . . .
C3A C 0.7234(4) 0.8095(4) 1.0279(3) 0.0525(9) Uani 1 1 d . . .
H3AA H 0.6355 0.8327 1.0616 0.063 Uiso 1 1 calc R . .
C4A C 0.8290(5) 0.8150(5) 1.0615(3) 0.0673(13) Uani 1 1 d . . .
H4AA H 0.8125 0.8431 1.1177 0.081 Uiso 1 1 calc R . .
C5A C 0.9557(5) 0.7809(6) 1.0152(4) 0.0742(15) Uani 1 1 d . . .
H5AA H 1.0263 0.7860 1.0395 0.089 Uiso 1 1 calc R . .
C6A C 0.9845(4) 0.7382(5) 0.9317(3) 0.0554(10) Uani 1 1 d . . .
C7A C 0.6301(4) 0.7649(4) 0.9072(3) 0.0502(9) Uani 1 1 d . . .
H7AA H 0.6685 0.7542 0.8432 0.060 Uiso 1 1 calc R . .
C8A C 0.5565(5) 0.6490(5) 0.9531(5) 0.0809(18) Uani 1 1 d . . .
H8AA H 0.6188 0.5714 0.9487 0.121 Uiso 1 1 calc R . .
H8AB H 0.4879 0.6419 0.9247 0.121 Uiso 1 1 calc R . .
H8AC H 0.5150 0.6586 1.0157 0.121 Uiso 1 1 calc R . .
C9A C 0.5362(5) 0.8877(5) 0.9127(4) 0.0621(12) Uani 1 1 d . . .
H9AA H 0.5858 0.9612 0.8818 0.093 Uiso 1 1 calc R . .
H9AB H 0.4956 0.8994 0.9750 0.093 Uiso 1 1 calc R . .
H9AC H 0.4666 0.8815 0.8849 0.093 Uiso 1 1 calc R . .
C10A C 1.1246(5) 0.6962(7) 0.8809(4) 0.0848(19) Uani 1 1 d . . .
H10A H 1.1196 0.6745 0.8233 0.102 Uiso 1 1 calc R . .
C11A C 1.1817(8) 0.5809(8) 0.9247(8) 0.174(6) Uani 1 1 d . . .
H11A H 1.1229 0.5125 0.9370 0.261 Uiso 1 1 calc R . .
H11B H 1.1923 0.5988 0.9805 0.261 Uiso 1 1 calc R . .
H11C H 1.2685 0.5535 0.8861 0.261 Uiso 1 1 calc R . .
C12A C 1.2123(9) 0.8048(10) 0.8583(8) 0.161(5) Uani 1 1 d . . .
H12A H 1.3024 0.7746 0.8261 0.242 Uiso 1 1 calc R . .
H12B H 1.2141 0.8342 0.9130 0.242 Uiso 1 1 calc R . .
H12C H 1.1771 0.8760 0.8212 0.242 Uiso 1 1 calc R . .
N2 N 0.7839(3) 0.6991(2) 0.67377(17) 0.0304(5) Uani 1 1 d . . .
C1B C 0.6656(3) 0.7424(3) 0.65338(19) 0.0266(6) Uani 1 1 d . . .
C2B C 0.5891(3) 0.6534(3) 0.6387(2) 0.0342(7) Uani 1 1 d . . .
C3B C 0.4761(4) 0.7022(4) 0.6122(3) 0.0482(9) Uani 1 1 d . . .
H3BA H 0.4233 0.6446 0.6014 0.058 Uiso 1 1 calc R . .
C4B C 0.4392(4) 0.8321(4) 0.6012(3) 0.0534(10) Uani 1 1 d . . .
H4BA H 0.3615 0.8632 0.5832 0.064 Uiso 1 1 calc R . .
C5B C 0.5150(4) 0.9176(3) 0.6165(3) 0.0439(8) Uani 1 1 d . . .
H5BA H 0.4889 1.0071 0.6078 0.053 Uiso 1 1 calc R . .
C6B C 0.6276(3) 0.8756(3) 0.6441(2) 0.0322(7) Uani 1 1 d . . .
C7B C 0.6256(4) 0.5106(3) 0.6547(3) 0.0416(8) Uani 1 1 d . . .
H7BA H 0.7169 0.4975 0.6624 0.050 Uiso 1 1 calc R . .
C8B C 0.6288(6) 0.4438(4) 0.5759(3) 0.0638(14) Uani 1 1 d . . .
H8BA H 0.6889 0.4845 0.5220 0.096 Uiso 1 1 calc R . .
H8BB H 0.5394 0.4513 0.5685 0.096 Uiso 1 1 calc R . .
H8BC H 0.6602 0.3529 0.5869 0.096 Uiso 1 1 calc R . .
C9B C 0.5336(6) 0.4494(4) 0.7388(3) 0.0638(12) Uani 1 1 d . . .
H9BA H 0.5333 0.4926 0.7886 0.096 Uiso 1 1 calc R . .
H9BB H 0.5641 0.3583 0.7500 0.096 Uiso 1 1 calc R . .
H9BC H 0.4436 0.4576 0.7323 0.096 Uiso 1 1 calc R . .
C10B C 0.7096(4) 0.9694(3) 0.6625(3) 0.0411(8) Uani 1 1 d . . .
H10B H 0.7454 0.9257 0.7126 0.049 Uiso 1 1 calc R . .
C11B C 0.6279(6) 1.0939(4) 0.6921(4) 0.0680(14) Uani 1 1 d . . .
H11D H 0.5521 1.0727 0.7430 0.102 Uiso 1 1 calc R . .
H11E H 0.5958 1.1424 0.6432 0.102 Uiso 1 1 calc R . .
H11F H 0.6836 1.1460 0.7089 0.102 Uiso 1 1 calc R . .
C12B C 0.8284(5) 0.9980(5) 0.5828(3) 0.0613(12) Uani 1 1 d . . .
H12D H 0.8781 0.9172 0.5652 0.092 Uiso 1 1 calc R . .
H12E H 0.8861 1.0491 0.5987 0.092 Uiso 1 1 calc R . .
H12F H 0.7974 1.0462 0.5334 0.092 Uiso 1 1 calc R . .
N3 N 0.9385(3) 0.4702(3) 0.73015(18) 0.0336(6) Uani 1 1 d . . .
C1 C 0.9166(3) 0.3437(3) 0.7641(2) 0.0277(6) Uani 1 1 d . . .
C2 C 0.8055(3) 0.3218(3) 0.8363(2) 0.0384(7) Uani 1 1 d . . .
H2A H 0.7483 0.3927 0.8592 0.046 Uiso 1 1 calc R . .
C3 C 0.7775(4) 0.1991(4) 0.8748(3) 0.0468(9) Uani 1 1 d . . .
H3B H 0.7014 0.1854 0.9237 0.056 Uiso 1 1 calc R . .
C4 C 0.8608(4) 0.0964(4) 0.8417(3) 0.0487(9) Uani 1 1 d . . .
H4A H 0.8433 0.0113 0.8684 0.058 Uiso 1 1 calc R . .
C5 C 0.9691(4) 0.1168(3) 0.7701(3) 0.0407(8) Uani 1 1 d . . .
H5A H 1.0243 0.0443 0.7480 0.049 Uiso 1 1 calc R . .
C6 C 1.0022(3) 0.2393(3) 0.7279(2) 0.0297(6) Uani 1 1 d . . .
C7 C 1.1219(3) 0.2588(3) 0.6466(2) 0.0389(7) Uani 1 1 d . . .
C8 C 1.0760(4) 0.3273(4) 0.5667(2) 0.0484(9) Uani 1 1 d . . .
H8A H 1.0280 0.4106 0.5803 0.073 Uiso 1 1 calc R . .
H8B H 1.0172 0.2746 0.5534 0.073 Uiso 1 1 calc R . .
H8C H 1.1533 0.3405 0.5153 0.073 Uiso 1 1 calc R . .
C9 C 1.1974(5) 0.1290(4) 0.6210(3) 0.0605(12) Uani 1 1 d . . .
H9A H 1.1375 0.0774 0.6078 0.091 Uiso 1 1 calc R . .
H9B H 1.2298 0.0828 0.6703 0.091 Uiso 1 1 calc R . .
H9C H 1.2727 0.1446 0.5685 0.091 Uiso 1 1 calc R . .
C10 C 1.2211(4) 0.3355(4) 0.6663(3) 0.0469(8) Uani 1 1 d . . .
H10C H 1.1770 0.4190 0.6824 0.070 Uiso 1 1 calc R . .
H10D H 1.2965 0.3484 0.6135 0.070 Uiso 1 1 calc R . .
H10E H 1.2529 0.2876 0.7155 0.070 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'
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'
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
N1 Re1 N2 111.46(13) . . ?
N1 Re1 N3 110.56(13) . . ?
N2 Re1 N3 111.62(12) . . ?
N1 Re1 Cl1 107.54(9) . . ?
N2 Re1 Cl1 107.37(8) . . ?
N3 Re1 Cl1 108.10(9) . . ?
C1A N1 Re1 172.4(2) . . ?
N1 C1A C2A 120.8(3) . . ?
N1 C1A C6A 116.8(3) . . ?
C2A C1A C6A 122.3(3) . . ?
C3A C2A C1A 118.1(3) . . ?
C3A C2A C7A 121.6(3) . . ?
C1A C2A C7A 120.4(3) . . ?
C4A C3A C2A 120.7(4) . . ?
C5A C4A C3A 120.9(4) . . ?
C4A C5A C6A 121.4(4) . . ?
C5A C6A C1A 116.5(4) . . ?
C5A C6A C10A 121.8(4) . . ?
C1A C6A C10A 121.7(4) . . ?
C8A C7A C2A 109.9(4) . . ?
C8A C7A C9A 111.0(4) . . ?
C2A C7A C9A 112.2(4) . . ?
C11A C10A C6A 113.2(6) . . ?
C11A C10A C12A 112.1(7) . . ?
C6A C10A C12A 111.3(6) . . ?
C1B N2 Re1 171.2(2) . . ?
N2 C1B C6B 118.6(3) . . ?
N2 C1B C2B 119.6(3) . . ?
C6B C1B C2B 121.7(3) . . ?
C3B C2B C1B 117.6(3) . . ?
C3B C2B C7B 121.1(3) . . ?
C1B C2B C7B 121.3(3) . . ?
C4B C3B C2B 121.3(3) . . ?
C3B C4B C5B 120.2(3) . . ?
C6B C5B C4B 121.5(3) . . ?
C5B C6B C1B 117.6(3) . . ?
C5B C6B C10B 121.5(3) . . ?
C1B C6B C10B 120.8(3) . . ?
C2B C7B C9B 111.4(3) . . ?
C2B C7B C8B 112.1(3) . . ?
C9B C7B C8B 110.5(3) . . ?
C12B C10B C6B 110.7(3) . . ?
C12B C10B C11B 111.2(4) . . ?
C6B C10B C11B 113.4(3) . . ?
C1 N3 Re1 160.8(2) . . ?
N3 C1 C2 117.4(3) . . ?
N3 C1 C6 122.1(3) . . ?
C2 C1 C6 120.5(3) . . ?
C3 C2 C1 121.1(3) . . ?
C4 C3 C2 119.3(4) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 123.2(3) . . ?
C5 C6 C1 115.8(3) . . ?
C5 C6 C7 121.9(3) . . ?
C1 C6 C7 122.2(3) . . ?
C8 C7 C6 110.1(3) . . ?
C8 C7 C10 110.9(3) . . ?
C6 C7 C10 110.3(3) . . ?
C8 C7 C9 107.1(3) . . ?
C6 C7 C9 111.4(3) . . ?
C10 C7 C9 107.0(3) . . ?
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 N1 1.744(3) . ?
Re1 N2 1.751(3) . ?
Re1 N3 1.757(3) . ?
Re1 Cl1 2.2990(8) . ?
N1 C1A 1.387(4) . ?
C1A C2A 1.399(5) . ?
C1A C6A 1.416(5) . ?
C2A C3A 1.385(5) . ?
C2A C7A 1.525(5) . ?
C3A C4A 1.388(7) . ?
C4A C5A 1.360(7) . ?
C5A C6A 1.411(6) . ?
C6A C10A 1.513(7) . ?
C7A C8A 1.512(7) . ?
C7A C9A 1.525(6) . ?
C10A C11A 1.451(10) . ?
C10A C12A 1.512(12) . ?
N2 C1B 1.385(4) . ?
C1B C6B 1.410(4) . ?
C1B C2B 1.416(4) . ?
C2B C3B 1.391(5) . ?
C2B C7B 1.508(4) . ?
C3B C4B 1.376(5) . ?
C4B C5B 1.386(6) . ?
C5B C6B 1.383(5) . ?
C6B C10B 1.524(5) . ?
C7B C9B 1.511(6) . ?
C7B C8B 1.532(6) . ?
C10B C12B 1.525(6) . ?
C10B C11B 1.539(5) . ?
N3 C1 1.384(4) . ?
C1 C2 1.398(4) . ?
C1 C6 1.417(4) . ?
C2 C3 1.375(5) . ?
C3 C4 1.377(6) . ?
C4 C5 1.371(6) . ?
C5 C6 1.400(4) . ?
C6 C7 1.532(5) . ?
C7 C8 1.530(5) . ?
C7 C10 1.545(5) . ?
C7 C9 1.547(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652726
