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#$Date: 2023-09-25 11:55:05 +0300 (Mon, 25 Sep 2023) $
#$Revision: 286506 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/75/8107537.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_8107537
loop_
_publ_author_name
'Ramoba, Lesetja V.'
'Alexander, Orbett T.'
'Malan, Frederick P.'
'Manicum, Amanda-Lee E.'
_publ_section_title
;
 The crystal structure of fac-tricarbonyl((pyridin-2-yl)methanamino-κ2
 N,N′)-((pyridin-2-yl)methanamino-\kN)rhenium(I) nitrate,
 C15H16O3N4Re
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              709
_journal_page_last               711
_journal_paper_doi               10.1515/ncrs-2023-0164
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C15 H16 N4 O3 Re, N O3'
_chemical_formula_sum            'C16 H13 N4 O6 Re'
_chemical_formula_weight         543.50
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                103.453(2)
_cell_angle_beta                 101.992(2)
_cell_angle_gamma                107.880(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4939(2)
_cell_length_b                   10.1316(2)
_cell_length_c                   13.8351(3)
_cell_measurement_reflns_used    26938
_cell_measurement_temperature    150.04(15)
_cell_measurement_theta_max      31.1870
_cell_measurement_theta_min      2.2950
_cell_volume                     926.98(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.04(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -22.00  42.00   0.50    0.06    --    4.46  85.00 116.00  128
  2  ω    -18.00  38.00   0.50    0.06    --    4.46 -99.00 120.00  112
  3  ω    -18.00  38.00   0.50    0.06    --    4.46 -99.00  60.00  112
  4  ω    -37.00  31.00   0.50    0.06    --    4.46 -85.00  -2.00  136
  5  ω    -18.00  38.00   0.50    0.06    --    4.46 -99.00 -90.00  112
  6  ω    -71.00  14.00   0.50    0.06    --    4.46 -19.00 -90.00  170
  7  ω    -78.00   9.00   0.50    0.06    --   -6.10 -57.00 -60.00  174
  8  ω    -79.00   6.00   0.50    0.06    --   -6.10 -37.00   0.00  170
  9  ω    -79.00   6.00   0.50    0.06    --   -6.10 -37.00  90.00  170
 10  ω    -18.00  27.00   0.50    0.06    --   -6.10 -99.00 -60.00   90
 11  ω    -18.00  27.00   0.50    0.06    --   -6.10 -99.00-150.00   90
 12  ω    -18.00  27.00   0.50    0.06    --   -6.10 -99.00-180.00   90
 13  ω    -18.00  59.00   0.50    0.06    --   -6.10  37.00-180.00  154
 14  ω    -18.00  67.00   0.50    0.06    --   -6.10  37.00  60.00  170
 15  ω    -32.00  42.00   0.50    0.06    --   -6.10  85.00 116.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0643978000
_diffrn_orient_matrix_UB_12      -0.0187332000
_diffrn_orient_matrix_UB_13      -0.0267032000
_diffrn_orient_matrix_UB_21      -0.0394549000
_diffrn_orient_matrix_UB_22      0.0233526000
_diffrn_orient_matrix_UB_23      -0.0411439000
_diffrn_orient_matrix_UB_31      0.0719549000
_diffrn_orient_matrix_UB_32      0.0715932000
_diffrn_orient_matrix_UB_33      0.0255166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.909
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.97a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       Block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.447
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0341
_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)+(0.0535P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4684
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0164_suppl_001.cif
_cod_data_source_block           am27_lt_auto
_cod_database_code               8107537
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N9(H9A,H9B), N27(H27A,H27B), C26(H26A,H26B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C24(H24), C22(H22), C25(H25), C23(H23)

;
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
C2 C 0.5542(6) 0.2674(4) 0.6564(3) 0.0263(8) Uani 1 1 d . . . . .
C3 C 0.4152(6) 0.1228(5) 0.6221(4) 0.0321(10) Uani 1 1 d . . . . .
H3 H 0.389983 0.059977 0.553967 0.039 Uiso 1 1 calc R . . . .
C4 C 0.3175(7) 0.0738(5) 0.6870(4) 0.0346(10) Uani 1 1 d . . . . .
H4 H 0.223945 -0.023494 0.664628 0.041 Uiso 1 1 calc R . . . .
C5 C 0.3553(6) 0.1673(4) 0.7868(4) 0.0318(9) Uani 1 1 d . . . . .
H5 H 0.289052 0.134969 0.833464 0.038 Uiso 1 1 calc R . . . .
C6 C 0.4910(6) 0.3076(4) 0.8158(3) 0.0256(8) Uani 1 1 d . . . . .
H6 H 0.516936 0.371776 0.883543 0.031 Uiso 1 1 calc R . . . .
C8 C 0.6604(6) 0.3271(4) 0.5870(3) 0.0285(9) Uani 1 1 d . . . . .
H8A H 0.700671 0.252123 0.547751 0.034 Uiso 1 1 calc R . . . .
H8B H 0.571018 0.350405 0.536040 0.034 Uiso 1 1 calc R . . . .
C15 C 1.0148(7) 0.5430(5) 0.8787(3) 0.0279(9) Uani 1 1 d . . . . .
C17 C 0.7459(6) 0.6605(4) 0.9177(3) 0.0261(8) Uani 1 1 d . . . . .
C19 C 1.0016(7) 0.7673(5) 0.8176(4) 0.0298(9) Uani 1 1 d . . . . .
C20 C 0.6238(7) 0.8696(5) 0.7543(4) 0.0356(11) Uani 1 1 d . . . . .
C22 C 0.8244(9) 1.0328(6) 0.6952(6) 0.0547(17) Uani 1 1 d . . . . .
H22 H 0.877147 1.052670 0.641082 0.066 Uiso 1 1 calc R . . . .
C23 C 0.8821(9) 1.1427(6) 0.7859(7) 0.064(2) Uani 1 1 d . . . . .
H23 H 0.973456 1.236760 0.794702 0.077 Uiso 1 1 calc R . . . .
C24 C 0.8070(11) 1.1166(7) 0.8654(7) 0.073(3) Uani 1 1 d . . . . .
H24 H 0.844003 1.192570 0.929305 0.088 Uiso 1 1 calc R . . . .
C25 C 0.6751(9) 0.9761(6) 0.8503(5) 0.0545(16) Uani 1 1 d . . . . .
H25 H 0.622018 0.954013 0.903831 0.065 Uiso 1 1 calc R . . . .
C26 C 0.4813(7) 0.7148(5) 0.7283(4) 0.0323(9) Uani 1 1 d . . . . .
H26A H 0.449452 0.698987 0.791693 0.039 Uiso 1 1 calc R . . . .
H26B H 0.357827 0.697795 0.675714 0.039 Uiso 1 1 calc R . . . .
N7 N 0.5891(5) 0.3581(4) 0.7521(3) 0.0213(7) Uani 1 1 d . . . . .
N9 N 0.8374(5) 0.4613(4) 0.6476(3) 0.0243(7) Uani 1 1 d . . . . .
H9A H 0.857639 0.521934 0.608376 0.029 Uiso 1 1 calc R . . . .
H9B H 0.944281 0.436088 0.661486 0.029 Uiso 1 1 calc R . . . .
N11 N 0.1137(5) 0.3339(4) 0.5232(3) 0.0317(8) Uani 1 1 d . . . . .
N27 N 0.5714(5) 0.6110(4) 0.6869(3) 0.0272(7) Uani 1 1 d . . . . .
H27A H 0.620875 0.640185 0.637285 0.033 Uiso 1 1 calc R . . . .
H27B H 0.472664 0.521922 0.653867 0.033 Uiso 1 1 calc R . . . .
N28 N 0.6960(6) 0.8964(4) 0.6774(4) 0.0409(9) Uani 1 1 d . . . . .
O10 O 0.1276(6) 0.3314(5) 0.6135(3) 0.0590(11) Uani 1 1 d . . . . .
O12 O -0.0461(5) 0.2904(5) 0.4542(3) 0.0582(11) Uani 1 1 d . . . . .
O13 O 0.2672(5) 0.3935(4) 0.5026(3) 0.0351(7) Uani 1 1 d . . . . .
O14 O 1.1457(5) 0.5279(4) 0.9301(3) 0.0408(8) Uani 1 1 d . . . . .
O16 O 0.7029(5) 0.7072(4) 0.9890(3) 0.0423(8) Uani 1 1 d . . . . .
O18 O 1.1243(5) 0.8797(4) 0.8349(3) 0.0497(10) Uani 1 1 d . . . . .
Re1 Re 0.80884(2) 0.57883(2) 0.79542(2) 0.01999(7) 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'
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
N7 Re1 N9 75.81(13) . .
N7 Re1 N27 83.27(14) . .
N9 Re1 N27 82.07(13) . .
C15 Re1 N7 95.63(16) . .
C15 Re1 N9 93.48(16) . .
C15 Re1 N27 175.55(14) . .
C15 Re1 C19 86.6(2) . .
C15 Re1 C17 90.49(19) . .
C19 Re1 N7 173.62(16) . .
C19 Re1 N9 98.12(18) . .
C19 Re1 N27 94.03(17) . .
C19 Re1 C17 89.39(19) . .
C17 Re1 N7 96.55(15) . .
C17 Re1 N9 171.69(15) . .
C17 Re1 N27 93.91(16) . .
C6 N7 Re1 124.2(3) . .
C2 N7 Re1 117.0(3) . .
C2 N7 C6 118.8(4) . .
C8 N9 Re1 112.4(2) . .
C26 N27 Re1 119.8(3) . .
O10 N11 O13 118.2(4) . .
O10 N11 O12 123.4(4) . .
O12 N11 O13 118.1(4) . .
O14 C15 Re1 176.8(4) . .
C20 N28 C22 117.6(6) . .
N7 C6 C5 122.9(4) . .
C6 C5 C4 118.3(4) . .
O18 C19 Re1 176.4(4) . .
O16 C17 Re1 178.1(4) . .
N7 C2 C3 120.8(4) . .
N7 C2 C8 117.6(4) . .
C3 C2 C8 121.5(4) . .
N28 C20 C26 114.4(4) . .
N28 C20 C25 122.6(5) . .
C25 C20 C26 122.9(6) . .
C3 C4 C5 119.6(4) . .
N27 C26 C20 109.3(4) . .
C4 C3 C2 119.7(4) . .
N9 C8 C2 111.4(3) . .
C23 C24 C25 118.8(6) . .
N28 C22 C23 123.6(7) . .
C20 C25 C24 118.0(7) . .
C22 C23 C24 119.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 N7 2.186(4) .
Re1 N9 2.202(3) .
Re1 N27 2.237(4) .
Re1 C15 1.908(5) .
Re1 C19 1.918(4) .
Re1 C17 1.921(4) .
N7 C6 1.352(5) .
N7 C2 1.344(5) .
O13 N11 1.249(5) .
O14 C15 1.159(6) .
O16 C17 1.144(5) .
N9 C8 1.486(5) .
O18 C19 1.157(6) .
N27 C26 1.485(5) .
N11 O10 1.239(5) .
N11 O12 1.243(5) .
N28 C20 1.334(7) .
N28 C22 1.350(7) .
C6 C5 1.376(6) .
C5 C4 1.395(6) .
C2 C3 1.411(6) .
C2 C8 1.488(6) .
C20 C26 1.509(7) .
C20 C25 1.394(7) .
C4 C3 1.359(7) .
C24 C25 1.399(10) .
C24 C23 1.377(12) .
C22 C23 1.353(10) .
loop_
_publcif_info_cif.paper_type
?
;
;
