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#$Date: 2022-03-09 12:30:40 +0200 (Wed, 09 Mar 2022) $
#$Revision: 273566 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/47/8104705.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_8104705
loop_
_publ_author_name
'Komane, Wesley K.'
'Mokolokolo, Pennie'
'Vatsha, Banele'
'Manicum, Amanda-Lee E.'
_publ_section_title
;
 The crystal structure of fac-tricarbonyl
 (N′-benzoyl-N,N-diphenylcarbamimidothioato-κ2
 S,O)-(pyrazole-\kN)rhenium(I) --- methanol (1/1) C26H23O4N4SRe
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              767
_journal_page_last               769
_journal_paper_doi               10.1515/ncrs-2021-0046
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C26 H19 N4 O4 Re S, C H4 O'
_chemical_formula_sum            'C27 H23 N4 O5 Re S'
_chemical_formula_weight         701.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                111.098(7)
_cell_angle_beta                 94.467(7)
_cell_angle_gamma                98.295(7)
_cell_formula_units_Z            2
_cell_length_a                   9.919(2)
_cell_length_b                   11.752(3)
_cell_length_c                   12.717(3)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.55
_cell_volume                     1355.0(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28629
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.416
_diffrn_reflns_theta_min         2.525
_exptl_absorpt_coefficient_mu    4.605
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1280 before and 0.0937 after correction.
The Ratio of minimum to maximum transmission is 0.7427.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0282P)²+2.8708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6176
_reflns_number_total             6727
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0046_suppl.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1354.9(5)
_cod_database_code               8104705
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.318
_shelx_estimated_absorpt_t_max   0.770
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.15615(2) 0.26486(2) 0.61077(2) 0.02059(6) Uani 1 1 d . . . . .
S1 S 0.13423(10) 0.46874(10) 0.74707(10) 0.0256(2) Uani 1 1 d . . . . .
O4 O 0.3664(3) 0.3055(3) 0.6821(3) 0.0266(6) Uani 1 1 d . . . . .
O2 O -0.1446(3) 0.2264(3) 0.5100(3) 0.0363(8) Uani 1 1 d . . . . .
O1 O 0.1892(4) 0.0175(3) 0.4294(3) 0.0473(10) Uani 1 1 d . . . . .
N3 N 0.4193(3) 0.5187(3) 0.7938(3) 0.0232(7) Uani 1 1 d . . . . .
O3 O 0.0642(4) 0.1328(4) 0.7692(3) 0.0426(9) Uani 1 1 d . . . . .
N1 N 0.2368(4) 0.3666(4) 0.5072(3) 0.0263(8) Uani 1 1 d . . . . .
N4 N 0.3080(3) 0.6801(3) 0.8412(3) 0.0214(7) Uani 1 1 d . . . . .
O9 O 0.5471(4) 0.1927(4) 0.4341(4) 0.0519(10) Uani 1 1 d . . . . .
N2 N 0.3377(4) 0.3371(4) 0.4425(4) 0.0357(9) Uani 1 1 d . . . . .
C2 C -0.0301(4) 0.2388(4) 0.5471(4) 0.0243(8) Uani 1 1 d . . . . .
C32 C 0.6289(4) 0.2788(4) 0.7371(4) 0.0238(8) Uani 1 1 d . . . . .
H32 H 0.566938 0.210060 0.682115 0.029 Uiso 1 1 calc R U . . .
C3 C 0.0987(5) 0.1825(4) 0.7086(4) 0.0287(9) Uani 1 1 d . . . . .
C33 C 0.7604(5) 0.2659(4) 0.7690(4) 0.0285(9) Uani 1 1 d . . . . .
H33 H 0.788788 0.188586 0.735104 0.034 Uiso 1 1 calc R U . . .
C7 C 0.4436(4) 0.4044(4) 0.7505(3) 0.0212(8) Uani 1 1 d . . . . .
C31 C 0.5870(4) 0.3918(4) 0.7851(3) 0.0207(8) Uani 1 1 d . . . . .
C11 C 0.1889(4) 0.7385(4) 0.8419(3) 0.0204(8) Uani 1 1 d . . . . .
C34 C 0.8517(5) 0.3657(5) 0.8506(4) 0.0325(10) Uani 1 1 d . . . . .
H34 H 0.941648 0.356410 0.873265 0.039 Uiso 1 1 calc R U . . .
C16 C 0.1444(5) 0.7616(4) 0.7470(4) 0.0279(9) Uani 1 1 d . . . . .
H16 H 0.190542 0.738956 0.681836 0.034 Uiso 1 1 calc R U . . .
C8 C 0.2972(4) 0.5551(4) 0.7921(3) 0.0202(8) Uani 1 1 d . . . . .
C1 C 0.1771(4) 0.1104(4) 0.4981(4) 0.0295(9) Uani 1 1 d . . . . .
C12 C 0.1242(5) 0.7729(4) 0.9379(4) 0.0296(9) Uani 1 1 d . . . . .
H12 H 0.157561 0.758404 1.003213 0.036 Uiso 1 1 calc R U . . .
C35 C 0.8098(5) 0.4785(5) 0.8982(5) 0.0376(11) Uani 1 1 d . . . . .
H35 H 0.872351 0.547556 0.952203 0.045 Uiso 1 1 calc R U . . .
C36 C 0.6770(5) 0.4915(4) 0.8675(4) 0.0311(10) Uani 1 1 d . . . . .
H36 H 0.647750 0.568217 0.902636 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1875(5) 0.4534(5) 0.4804(5) 0.0365(11) Uani 1 1 d . . . . .
H00Q H 0.114482 0.491746 0.512520 0.044 Uiso 1 1 calc R U . . .
C15 C 0.0303(5) 0.8188(5) 0.7490(4) 0.0378(12) Uani 1 1 d . . . . .
H15 H -0.001597 0.835238 0.684432 0.045 Uiso 1 1 calc R U . . .
C5 C 0.2571(6) 0.4808(5) 0.3988(5) 0.0424(12) Uani 1 1 d . . . . .
H00S H 0.241245 0.538965 0.365348 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4346(4) 0.7584(4) 0.9072(4) 0.0243(9) Uani 1 1 d . . . . .
C14 C -0.0360(5) 0.8513(5) 0.8423(5) 0.0400(12) Uani 1 1 d . . . . .
H14 H -0.114006 0.889657 0.842126 0.048 Uiso 1 1 calc R U . . .
C26 C 0.4815(5) 0.7536(4) 1.0109(4) 0.0305(10) Uani 1 1 d . . . . .
H26 H 0.431680 0.696680 1.037661 0.037 Uiso 1 1 calc R U . . .
C22 C 0.5071(4) 0.8416(4) 0.8684(4) 0.0287(9) Uani 1 1 d . . . . .
H22 H 0.475438 0.845396 0.797456 0.034 Uiso 1 1 calc R U . . .
C13 C 0.0100(5) 0.8288(5) 0.9381(5) 0.0365(11) Uani 1 1 d . . . . .
H13 H -0.036551 0.851448 1.003008 0.044 Uiso 1 1 calc R U . . .
C6 C 0.3530(6) 0.4059(5) 0.3774(5) 0.0458(13) Uani 1 1 d . . . . .
H00Y H 0.418534 0.402692 0.326200 0.055 Uiso 1 1 calc R U . . .
C25 C 0.6010(5) 0.8318(5) 1.0752(4) 0.0356(11) Uani 1 1 d . . . . .
H25 H 0.633182 0.828552 1.146242 0.043 Uiso 1 1 calc R U . . .
C9 C 0.5515(7) 0.0657(6) 0.3820(6) 0.0563(16) Uani 1 1 d . . . . .
H93 H 0.627847 0.055567 0.336982 0.084 Uiso 1 1 calc R U . . .
H91 H 0.464686 0.022111 0.332147 0.084 Uiso 1 1 calc R U . . .
H92 H 0.565101 0.031071 0.440745 0.084 Uiso 1 1 calc R U . . .
C23 C 0.6269(5) 0.9196(5) 0.9345(5) 0.0393(12) Uani 1 1 d . . . . .
H23 H 0.676935 0.977127 0.908576 0.047 Uiso 1 1 calc R U . . .
C24 C 0.6735(5) 0.9144(5) 1.0366(5) 0.0393(12) Uani 1 1 d . . . . .
H24 H 0.755806 0.967739 1.080758 0.047 Uiso 1 1 calc R U . . .
H00B H 0.394(6) 0.287(6) 0.457(5) 0.049(17) Uiso 1 1 d . . . . .
H94 H 0.624(12) 0.254(12) 0.494(10) 0.16(5) Uiso 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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C2 Re1 C3 89.11(18) . .
C2 Re1 C1 90.37(19) . .
C3 Re1 C1 90.5(2) . .
C2 Re1 O4 176.38(14) . .
C3 Re1 O4 93.57(16) . .
C1 Re1 O4 92.04(15) . .
C2 Re1 N1 94.95(16) . .
C3 Re1 N1 175.64(16) . .
C1 Re1 N1 91.07(18) . .
O4 Re1 N1 82.30(13) . .
C2 Re1 S1 89.76(13) . .
C3 Re1 S1 93.00(14) . .
C1 Re1 S1 176.50(15) . .
O4 Re1 S1 87.67(8) . .
N1 Re1 S1 85.43(10) . .
C8 S1 Re1 106.74(14) . .
C7 O4 Re1 132.4(3) . .
C7 N3 C8 127.5(4) . .
C4 N1 N2 105.5(4) . .
C4 N1 Re1 129.3(3) . .
N2 N1 Re1 124.5(3) . .
C8 N4 C21 121.1(3) . .
C8 N4 C11 121.4(3) . .
C21 N4 C11 117.0(3) . .
N1 N2 C6 111.0(4) . .
O2 C2 Re1 178.0(4) . .
C33 C32 C31 120.2(4) . .
O3 C3 Re1 179.5(4) . .
C32 C33 C34 120.4(4) . .
O4 C7 N3 130.2(4) . .
O4 C7 C31 115.5(3) . .
N3 C7 C31 114.3(3) . .
C32 C31 C36 119.7(4) . .
C32 C31 C7 119.7(4) . .
C36 C31 C7 120.6(4) . .
C12 C11 C16 121.3(4) . .
C12 C11 N4 119.5(4) . .
C16 C11 N4 119.1(4) . .
C35 C34 C33 119.3(4) . .
C11 C16 C15 118.6(4) . .
N3 C8 N4 112.9(3) . .
N3 C8 S1 130.1(3) . .
N4 C8 S1 116.8(3) . .
O1 C1 Re1 179.4(5) . .
C11 C12 C13 119.3(4) . .
C34 C35 C36 120.5(5) . .
C35 C36 C31 119.8(4) . .
N1 C4 C5 111.1(4) . .
C14 C15 C16 120.8(5) . .
C6 C5 C4 105.0(5) . .
C22 C21 C26 120.1(4) . .
C22 C21 N4 119.6(4) . .
C26 C21 N4 120.3(4) . .
C15 C14 C13 120.4(4) . .
C25 C26 C21 119.9(5) . .
C21 C22 C23 119.1(5) . .
C12 C13 C14 119.6(4) . .
N2 C6 C5 107.4(5) . .
C24 C25 C26 120.2(5) . .
C24 C23 C22 120.8(5) . .
C23 C24 C25 120.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C2 1.894(4) .
Re1 C3 1.905(5) .
Re1 C1 1.917(5) .
Re1 O4 2.123(3) .
Re1 N1 2.196(4) .
Re1 S1 2.4518(12) .
S1 C8 1.713(4) .
O4 C7 1.266(5) .
O2 C2 1.163(5) .
O1 C1 1.156(6) .
N3 C7 1.322(5) .
N3 C8 1.342(5) .
O3 C3 1.166(6) .
N1 C4 1.329(6) .
N1 N2 1.350(5) .
N4 C8 1.358(5) .
N4 C21 1.441(5) .
N4 C11 1.449(5) .
O9 C9 1.406(7) .
N2 C6 1.352(7) .
C32 C33 1.381(6) .
C32 C31 1.387(6) .
C33 C34 1.394(7) .
C7 C31 1.500(5) .
C31 C36 1.391(6) .
C11 C12 1.381(6) .
C11 C16 1.382(6) .
C34 C35 1.384(7) .
C16 C15 1.395(6) .
C12 C13 1.390(6) .
C35 C36 1.390(6) .
C4 C5 1.395(7) .
C15 C14 1.362(7) .
C5 C6 1.365(8) .
C21 C22 1.385(6) .
C21 C26 1.387(6) .
C14 C13 1.394(8) .
C26 C25 1.382(7) .
C22 C23 1.391(7) .
C25 C24 1.378(8) .
C23 C24 1.369(8) .
