The crystal structure of fac-tricarbonyl(2-pyridin-2-yl-quinoline-κ2 N,N′)-(pyrazole-κN)rhenium(I)nitrate, C20H14N4O3ReNO3
Sithole, Sibusiso A.; Malan, Federick P.; Katerere, David R.; Manicum, Amanda-Lee E.; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 685–687; doi:10.1515/ncrs-2023-0152

data_8107531
_publ_section_title
;
 The crystal structure of fac-tricarbonyl(2-pyridin-2-yl-quinoline-\k2
 N,N&#x2032;)-(pyrazole-\kN)rhenium(I)nitrate, C20H14N4O3ReNO3
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              685
_journal_page_last               687
_journal_paper_doi               10.1515/ncrs-2023-0152
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C20 H14 N4 O3 Re, N O3'
_chemical_formula_sum            'C20 H14 N5 O6 Re'
_chemical_formula_weight         606.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9572(2)
_cell_length_b                   9.1568(2)
_cell_length_c                   17.3658(3)
_cell_measurement_reflns_used    23205
_cell_measurement_temperature    153.76(10)
_cell_measurement_theta_max      31.1710
_cell_measurement_theta_min      2.5280
_cell_volume                     2043.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      153.76(10)
_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 0.843
_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    -21.00  66.00   0.50    0.15    --   -6.08  57.00  30.00  174
  2  \w     -8.00  69.00   0.50    0.15    --   -6.08  21.00 126.00  154
  3  \w     -5.00  20.00   0.50    0.15    --   -6.08  19.00   0.00   50
  4  \w     -5.00  69.00   0.50    0.15    --   -6.08  19.00 -60.00  148
  5  \w     -5.00  69.00   0.50    0.15    --   -6.08  19.00-180.00  148
  6  \w    -81.00   6.00   0.50    0.15    --   -6.08 -21.00 -40.00  174
  7  \w    -18.00  27.00   0.50    0.15    --   -6.08 -99.00 -90.00   90
;
_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      0.0446273000
_diffrn_orient_matrix_UB_12      0.0158973000
_diffrn_orient_matrix_UB_13      0.0267362000
_diffrn_orient_matrix_UB_21      -0.0323041000
_diffrn_orient_matrix_UB_22      0.0145425000
_diffrn_orient_matrix_UB_23      0.0291705000
_diffrn_orient_matrix_UB_31      0.0032209000
_diffrn_orient_matrix_UB_32      -0.0743939000
_diffrn_orient_matrix_UB_33      0.0114051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33676
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.950
_diffrn_reflns_theta_min         2.365
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       blade
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4763
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0152_suppl_001.cif
_cod_data_source_block           shelx
_cod_database_code               8107531
_shelx_res_checksum              77641
_shelx_hkl_checksum              97152