The crystal structure of fac-tricarbonyl((pyridin-2-yl)methanamino-κ2 N,N′)-((pyridin-2-yl)methanamino-κN)rhenium(I) nitrate, C15H16O3N4Re
Ramoba, Lesetja V.; Alexander, Orbett T.; Malan, Frederick P.; Manicum, Amanda-Lee E.; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 709–711; doi:10.1515/ncrs-2023-0164

data_8107537
_publ_section_title
;
 The crystal structure of fac-tricarbonyl((pyridin-2-yl)methanamino-\k2
 N,N&#x2032;)-((pyridin-2-yl)methanamino-\kN)rhenium(I) nitrate,
 C15H16O3N4Re
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -22.00  42.00   0.50    0.06    --    4.46  85.00 116.00  128
  2  \w    -18.00  38.00   0.50    0.06    --    4.46 -99.00 120.00  112
  3  \w    -18.00  38.00   0.50    0.06    --    4.46 -99.00  60.00  112
  4  \w    -37.00  31.00   0.50    0.06    --    4.46 -85.00  -2.00  136
  5  \w    -18.00  38.00   0.50    0.06    --    4.46 -99.00 -90.00  112
  6  \w    -71.00  14.00   0.50    0.06    --    4.46 -19.00 -90.00  170
  7  \w    -78.00   9.00   0.50    0.06    --   -6.10 -57.00 -60.00  174
  8  \w    -79.00   6.00   0.50    0.06    --   -6.10 -37.00   0.00  170
  9  \w    -79.00   6.00   0.50    0.06    --   -6.10 -37.00  90.00  170
 10  \w    -18.00  27.00   0.50    0.06    --   -6.10 -99.00 -60.00   90
 11  \w    -18.00  27.00   0.50    0.06    --   -6.10 -99.00-150.00   90
 12  \w    -18.00  27.00   0.50    0.06    --   -6.10 -99.00-180.00   90
 13  \w    -18.00  59.00   0.50    0.06    --   -6.10  37.00-180.00  154
 14  \w    -18.00  67.00   0.50    0.06    --   -6.10  37.00  60.00  170
 15  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0535P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0164_suppl_001.cif
_cod_data_source_block           am27_lt_auto
_cod_database_code               8107537
_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)

;
_shelx_res_checksum              92705
_shelx_hkl_checksum              45262