Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand
Valdivieso, Jorge P.; Erickson, Alexander N.; Gardinier, James R.; RSC Advances 14 (2024) 31502–31516; doi:10.1039/D4RA05287K

data_7249432
_publ_section_title
;
 Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              31502
_journal_page_last               31516
_journal_paper_doi               10.1039/D4RA05287K
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C31 H28 N5 O2 P Re, C F3 O3 S'
_chemical_formula_sum            'C32 H28 F3 N5 O5 P Re S'
_chemical_formula_weight         868.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.962(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6364(3)
_cell_length_b                   12.9137(2)
_cell_length_c                   16.6780(3)
_cell_measurement_reflns_used    12601
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.5300
_cell_measurement_theta_min      4.4170
_cell_volume                     3323.04(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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    -67.00  32.00   1.00    1.00    --  -42.46  37.00 -30.00   99
  2  \w    -92.00  -2.00   1.00    1.00    --  -42.46 125.00 -30.00   90
  3  \w     23.00  98.00   1.00    1.00    --   42.46-125.00-180.00   75
  4  \w     17.00 110.00   1.00    2.50    --  100.00 -94.00-120.00   93
  5  \w     94.00 173.00   1.00    2.50    --  100.00 125.00-150.00   79
  6  \w     27.00 118.00   1.00    2.50    --  100.00-125.00-150.00   91
  7  \w     72.00 176.00   1.00    2.50    --  100.00  30.00 120.00  104
  8  \w     47.00 178.00   1.00    2.50    --  100.00  15.00  30.00  131
  9  \w     27.00 126.00   1.00    2.50    --  100.00 -45.00 -60.00   99
 10  \w     18.00 153.00   1.00    2.50    --  100.00 -15.00 150.00  135
 11  \w   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00  30.00  109
 12  \w     10.00 119.00   1.00    1.00    --   42.46  77.00 -90.00  109
 13  \w     14.00 116.00   1.00    1.00    --   42.46  57.00-180.00  102
 14  \w     71.00 132.00   1.00    2.50    --  100.00  61.00 150.00   61
 15  \w     47.00 178.00   1.00    2.50    --  100.00  15.00 -90.00  131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517969000
_diffrn_orient_matrix_UB_12      -0.0866965000
_diffrn_orient_matrix_UB_13      0.0222580000
_diffrn_orient_matrix_UB_21      0.0821701000
_diffrn_orient_matrix_UB_22      -0.0334554000
_diffrn_orient_matrix_UB_23      0.0763169000
_diffrn_orient_matrix_UB_31      -0.0231255000
_diffrn_orient_matrix_UB_32      0.0747272000
_diffrn_orient_matrix_UB_33      0.0601147000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.607
_diffrn_reflns_theta_min         4.460
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.766
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.142
_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     436
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0501P)^2^+1.8456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5398
_reflns_number_total             6303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           3-Re_gard25u
_cod_database_code               7249432
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C32H25N5F3O5PSRe
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C7(H7)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
1.c Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C47(H47a,H47b,H47c), C16(H16a,H16b,H16c)
;
_shelx_res_checksum              69026
_shelx_hkl_checksum              58509
_olex2_submission_original_sample_id gard25u
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.039
_oxdiff_exptl_absorpt_empirical_full_min 0.636