#------------------------------------------------------------------------------
#$Date: 2018-09-08 23:21:46 +0300 (Sat, 08 Sep 2018) $
#$Revision: 210586 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/48/7104815.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_7104815
loop_
_publ_author_name
'Braband, Henrik'
'Abram, Ulrich'
_publ_section_title
;
 Stable nitridorhenium(V) complexes with an N-heterocyclic carbene
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   19
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2436
_journal_page_last               2437
_journal_paper_doi               10.1039/b307216a
_journal_year                    2003
_chemical_formula_sum            'C36 H37 Cl2 N4 P2 Re'
_chemical_formula_weight         844.74
_chemical_name_systematic
;
Dichlorobis(dimethylphenylphosphine)(1,3,4-triphenyl-1,2,4-triazol-5-ylidene)
nitridorhenium(V)
;
_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                 113.48(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.825(2)
_cell_length_b                   31.595(3)
_cell_length_c                   11.319(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.55
_cell_measurement_theta_min      6.03
_cell_volume                     3550.6(11)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        HELENA
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CAD4 ENRAF NONIUS'
_diffrn_measurement_method       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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.1783
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6427
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 3600
_diffrn_standards_interval_time  500
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.694
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_correction_T_min  0.8321
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0574P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                2836
_reflns_number_total             5500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307216a.txt
_cod_data_source_block           rencarbenep2cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-Scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7104815
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.66038(5) 0.117751(18) 0.36491(6) 0.0481(2) Uani 1 1 d . . .
N10 N 0.7529(9) 0.1596(3) 0.4773(13) 0.076(4) Uani 1 1 d . . .
Cl1 Cl 0.7758(4) 0.10599(16) 0.2207(4) 0.0939(16) Uani 1 1 d . . .
Cl2 Cl 0.5217(4) 0.05106(12) 0.2823(4) 0.0786(12) Uani 1 1 d . . .
C1 C 0.5331(13) 0.1567(4) 0.2053(13) 0.045(3) Uani 1 1 d . . .
C2 C 0.3795(13) 0.1851(4) 0.0211(13) 0.048(3) Uani 1 1 d . . .
N1 N 0.4346(10) 0.1472(3) 0.0835(10) 0.048(3) Uani 1 1 d . . .
N2 N 0.5295(10) 0.1996(4) 0.2041(11) 0.053(3) Uani 1 1 d . . .
N3 N 0.4333(10) 0.2178(3) 0.0924(11) 0.053(3) Uani 1 1 d . . .
C11 C 0.3938(13) 0.1058(4) 0.0177(13) 0.050(4) Uani 1 1 d . . .
C12 C 0.2718(14) 0.0925(5) -0.0016(15) 0.067(4) Uani 1 1 d . . .
H12 H 0.2165 0.1070 0.0299 0.080 Uiso 1 1 calc R . .
C13 C 0.2322(19) 0.0561(6) -0.0707(17) 0.085(6) Uani 1 1 d . . .
H13 H 0.1460 0.0463 -0.0864 0.102 Uiso 1 1 calc R . .
C14 C 0.305(3) 0.0332(6) -0.1179(18) 0.112(9) Uani 1 1 d . . .
H14 H 0.2721 0.0085 -0.1643 0.134 Uiso 1 1 calc R . .
C15 C 0.425(2) 0.0475(7) -0.0951(18) 0.104(7) Uani 1 1 d . . .
H15 H 0.4800 0.0324 -0.1258 0.125 Uiso 1 1 calc R . .
C16 C 0.4759(16) 0.0859(5) -0.0239(15) 0.066(4) Uani 1 1 d . . .
H16 H 0.5616 0.0961 -0.0082 0.079 Uiso 1 1 calc R . .
C21 C 0.6176(14) 0.2295(5) 0.2953(13) 0.053(4) Uani 1 1 d . . .
C22 C 0.7420(15) 0.2314(5) 0.3056(15) 0.070(4) Uani 1 1 d . . .
H22 H 0.7758 0.2139 0.2594 0.084 Uiso 1 1 calc R . .
C23 C 0.8219(15) 0.2629(6) 0.3951(17) 0.078(5) Uani 1 1 d . . .
H23 H 0.9131 0.2643 0.4119 0.094 Uiso 1 1 calc R . .
C24 C 0.773(2) 0.2907(5) 0.4563(18) 0.090(6) Uani 1 1 d . . .
H24 H 0.8301 0.3110 0.5101 0.108 Uiso 1 1 calc R . .
C25 C 0.6488(18) 0.2896(5) 0.4419(18) 0.087(6) Uani 1 1 d . . .
H25 H 0.6137 0.3081 0.4845 0.104 Uiso 1 1 calc R . .
C26 C 0.5703(15) 0.2582(5) 0.3563(14) 0.062(4) Uani 1 1 d . . .
H26 H 0.4792 0.2570 0.3406 0.075 Uiso 1 1 calc R . .
C31 C 0.2745(14) 0.1860(4) -0.1155(15) 0.056(4) Uani 1 1 d . . .
C32 C 0.1569(18) 0.2026(5) -0.1359(17) 0.079(5) Uani 1 1 d . . .
H32 H 0.1377 0.2122 -0.0674 0.095 Uiso 1 1 calc R . .
C33 C 0.0566(17) 0.2058(6) -0.268(2) 0.097(6) Uani 1 1 d . . .
H33 H -0.0275 0.2173 -0.2830 0.117 Uiso 1 1 calc R . .
C34 C 0.085(2) 0.1918(6) -0.372(2) 0.098(6) Uani 1 1 d . . .
H34 H 0.0196 0.1949 -0.4555 0.117 Uiso 1 1 calc R . .
C35 C 0.1999(17) 0.1747(6) -0.3555(17) 0.088(6) Uani 1 1 d . . .
H35 H 0.2185 0.1642 -0.4234 0.105 Uiso 1 1 calc R . .
C36 C 0.2947(15) 0.1732(5) -0.2260(15) 0.075(5) Uani 1 1 d . . .
H36 H 0.3796 0.1627 -0.2122 0.090 Uiso 1 1 calc R . .
P1 P 0.8207(4) 0.06852(13) 0.5183(4) 0.0576(11) Uani 1 1 d . . .
C41 C 0.8298(14) 0.0623(5) 0.6867(15) 0.058(4) Uani 1 1 d . . .
C42 C 0.8648(16) 0.0955(5) 0.7762(17) 0.084(6) Uani 1 1 d . . .
H42 H 0.8881 0.1218 0.7544 0.101 Uiso 1 1 calc R . .
C43 C 0.8646(19) 0.0886(8) 0.9062(19) 0.107(7) Uani 1 1 d . . .
H43 H 0.8920 0.1103 0.9669 0.129 Uiso 1 1 calc R . .
C44 C 0.825(3) 0.0509(9) 0.937(2) 0.127(9) Uani 1 1 d . . .
H44 H 0.8204 0.0463 1.0161 0.152 Uiso 1 1 calc R . .
C45 C 0.791(3) 0.0206(9) 0.846(3) 0.169(12) Uani 1 1 d . . .
H45 H 0.7662 -0.0057 0.8655 0.203 Uiso 1 1 calc R . .
C46 C 0.792(2) 0.0261(7) 0.725(2) 0.109(7) Uani 1 1 d . . .
H46 H 0.7653 0.0036 0.6673 0.131 Uiso 1 1 calc R . .
C47 C 0.9831(14) 0.0852(5) 0.5482(17) 0.098(6) Uani 1 1 d . . .
H47A H 0.9959 0.1134 0.5820 0.147 Uiso 1 1 calc R . .
H47B H 0.9967 0.0847 0.4694 0.147 Uiso 1 1 calc R . .
H47C H 1.0467 0.0666 0.6096 0.147 Uiso 1 1 calc R . .
C48 C 0.8173(16) 0.0157(4) 0.4575(16) 0.090(6) Uani 1 1 d . . .
H48A H 0.7304 0.0033 0.4382 0.135 Uiso 1 1 calc R . .
H48B H 0.8852 -0.0012 0.5213 0.135 Uiso 1 1 calc R . .
H48C H 0.8345 0.0167 0.3807 0.135 Uiso 1 1 calc R . .
P2 P 0.5185(4) 0.12142(15) 0.4818(4) 0.0605(10) Uani 1 1 d . . .
C51 C 0.3492(13) 0.1318(4) 0.3775(13) 0.052(4) Uani 1 1 d . . .
C52 C 0.3108(15) 0.1742(5) 0.3438(17) 0.080(5) Uani 1 1 d . . .
H52 H 0.3738 0.1960 0.3721 0.096 Uiso 1 1 calc R . .
C53 C 0.179(2) 0.1826(7) 0.269(2) 0.114(8) Uani 1 1 d . . .
H53 H 0.1504 0.2100 0.2416 0.137 Uiso 1 1 calc R . .
C54 C 0.094(2) 0.1499(10) 0.237(2) 0.124(10) Uani 1 1 d . . .
H54 H 0.0022 0.1552 0.1929 0.149 Uiso 1 1 calc R . .
C55 C 0.134(2) 0.1113(9) 0.264(2) 0.137(10) Uani 1 1 d . . .
H55 H 0.0716 0.0895 0.2320 0.164 Uiso 1 1 calc R . .
C56 C 0.2598(16) 0.1015(5) 0.3366(17) 0.079(5) Uani 1 1 d . . .
H56 H 0.2848 0.0735 0.3583 0.095 Uiso 1 1 calc R . .
C57 C 0.5089(16) 0.0781(6) 0.5836(17) 0.110(7) Uani 1 1 d . . .
H57A H 0.5980 0.0709 0.6436 0.165 Uiso 1 1 calc R . .
H57B H 0.4681 0.0540 0.5310 0.165 Uiso 1 1 calc R . .
H57C H 0.4556 0.0867 0.6299 0.165 Uiso 1 1 calc R . .
C58 C 0.5617(15) 0.1653(6) 0.6015(17) 0.117(8) Uani 1 1 d . . .
H58A H 0.6532 0.1621 0.6624 0.176 Uiso 1 1 calc R . .
H58B H 0.5026 0.1644 0.6460 0.176 Uiso 1 1 calc R . .
H58C H 0.5517 0.1919 0.5578 0.176 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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
N10 Re1 C1 99.1(5) . . ?
N10 Re1 P2 82.8(4) . . ?
C1 Re1 P2 95.6(3) . . ?
N10 Re1 Cl1 106.9(4) . . ?
C1 Re1 Cl1 81.6(3) . . ?
P2 Re1 Cl1 170.23(16) . . ?
N10 Re1 P1 85.9(3) . . ?
C1 Re1 P1 169.7(3) . . ?
P2 Re1 P1 93.91(14) . . ?
Cl1 Re1 P1 88.32(15) . . ?
N10 Re1 Cl2 159.1(4) . . ?
C1 Re1 Cl2 94.5(4) . . ?
P2 Re1 Cl2 80.13(15) . . ?
Cl1 Re1 Cl2 90.71(16) . . ?
P1 Re1 Cl2 83.25(14) . . ?
N2 C1 N1 101.4(11) . . ?
N2 C1 Re1 125.7(10) . . ?
N1 C1 Re1 132.9(9) . . ?
N3 C2 N1 111.9(11) . . ?
N3 C2 C31 126.1(12) . . ?
N1 C2 C31 121.9(13) . . ?
C2 N1 C1 108.5(11) . . ?
C2 N1 C11 121.4(11) . . ?
C1 N1 C11 130.0(11) . . ?
C1 N2 N3 115.2(11) . . ?
C1 N2 C21 129.7(12) . . ?
N3 N2 C21 114.8(11) . . ?
C2 N3 N2 102.9(10) . . ?
C12 C11 C16 124.1(14) . . ?
C12 C11 N1 116.3(13) . . ?
C16 C11 N1 119.5(13) . . ?
C11 C12 C13 115.5(16) . . ?
C14 C13 C12 126.1(19) . . ?
C15 C14 C13 116.0(19) . . ?
C14 C15 C16 122(2) . . ?
C11 C16 C15 116.2(16) . . ?
C22 C21 C26 120.7(15) . . ?
C22 C21 N2 117.2(14) . . ?
C26 C21 N2 121.6(13) . . ?
C21 C22 C23 113.7(15) . . ?
C24 C23 C22 124.2(15) . . ?
C25 C24 C23 121.4(18) . . ?
C24 C25 C26 114.8(18) . . ?
C21 C26 C25 124.9(15) . . ?
C32 C31 C36 116.2(15) . . ?
C32 C31 C2 118.0(16) . . ?
C36 C31 C2 125.6(13) . . ?
C31 C32 C33 118.9(17) . . ?
C34 C33 C32 121.1(16) . . ?
C35 C34 C33 121.6(19) . . ?
C34 C35 C36 114.9(18) . . ?
C31 C36 C35 127.1(15) . . ?
C47 P1 C48 102.7(8) . . ?
C47 P1 C41 101.3(8) . . ?
C48 P1 C41 106.0(8) . . ?
C47 P1 Re1 108.7(6) . . ?
C48 P1 Re1 114.5(6) . . ?
C41 P1 Re1 121.3(5) . . ?
C46 C41 C42 115.7(17) . . ?
C46 C41 P1 121.1(15) . . ?
C42 C41 P1 123.0(13) . . ?
C41 C42 C43 120.0(17) . . ?
C44 C43 C42 120(2) . . ?
C45 C44 C43 116(2) . . ?
C44 C45 C46 124(3) . . ?
C41 C46 C45 123(2) . . ?
C51 P2 C57 104.9(7) . . ?
C51 P2 C58 103.9(7) . . ?
C57 P2 C58 99.2(9) . . ?
C51 P2 Re1 111.2(5) . . ?
C57 P2 Re1 121.6(6) . . ?
C58 P2 Re1 114.0(6) . . ?
C56 C51 C52 120.2(14) . . ?
C56 C51 P2 121.6(12) . . ?
C52 C51 P2 118.2(11) . . ?
C53 C52 C51 118.4(17) . . ?
C54 C53 C52 117.4(19) . . ?
C55 C54 C53 122(2) . . ?
C54 C55 C56 122(2) . . ?
C51 C56 C55 119.0(17) . . ?
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 N10 1.831(12) . ?
Re1 C1 2.167(14) . ?
Re1 P2 2.396(4) . ?
Re1 Cl1 2.448(4) . ?
Re1 P1 2.459(4) . ?
Re1 Cl2 2.540(4) . ?
C1 N2 1.356(15) . ?
C1 N1 1.400(15) . ?
C2 N3 1.298(15) . ?
C2 N1 1.397(15) . ?
C2 C31 1.510(18) . ?
N1 C11 1.482(15) . ?
N2 N3 1.401(13) . ?
N2 C21 1.443(16) . ?
C11 C12 1.320(17) . ?
C11 C16 1.320(17) . ?
C12 C13 1.36(2) . ?
C13 C14 1.33(2) . ?
C14 C15 1.30(3) . ?
C15 C16 1.44(2) . ?
C21 C22 1.306(17) . ?
C21 C26 1.358(18) . ?
C22 C23 1.44(2) . ?
C23 C24 1.35(2) . ?
C24 C25 1.29(2) . ?
C25 C26 1.41(2) . ?
C31 C32 1.311(19) . ?
C31 C36 1.41(2) . ?
C32 C33 1.46(2) . ?
C33 C34 1.41(2) . ?
C34 C35 1.30(2) . ?
C35 C36 1.42(2) . ?
P1 C47 1.735(14) . ?
P1 C48 1.801(14) . ?
P1 C41 1.879(16) . ?
C41 C46 1.34(2) . ?
C41 C42 1.40(2) . ?
C42 C43 1.49(2) . ?
C43 C44 1.36(3) . ?
C44 C45 1.35(3) . ?
C45 C46 1.38(3) . ?
P2 C51 1.771(13) . ?
P2 C57 1.818(15) . ?
P2 C58 1.863(16) . ?
C51 C56 1.309(18) . ?
C51 C52 1.410(18) . ?
C52 C53 1.36(2) . ?
C53 C54 1.34(3) . ?
C54 C55 1.29(3) . ?
C55 C56 1.32(2) . ?
