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_7249434
_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         'C28 H25 F3 Mn0.5 N4 O4 P S'
_chemical_formula_sum            'C28 H25 F3 Mn0.5 N4 O4 P S'
_chemical_formula_weight         629.02
_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     direct
_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                64.443(3)
_cell_angle_beta                 85.597(3)
_cell_angle_gamma                88.991(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3815(3)
_cell_length_b                   12.9857(4)
_cell_length_c                   13.0750(5)
_cell_measurement_reflns_used    11411
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      70.5590
_cell_measurement_theta_min      3.9770
_cell_volume                     1432.56(9)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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   -115.00 -67.00   1.00    1.98    --  -42.46-134.00 106.00   48
  2  \w    -67.00  32.00   1.00    1.98    --  -42.46  37.00 120.00   99
  3  \w   -117.00 -18.00   1.00    1.98    --  -42.46 -37.00 -60.00   99
  4  \w     18.00 117.00   1.00    1.98    --   42.46  37.00-180.00   99
  5  \w     29.00 104.00   1.00    1.98    --   42.46-135.00 -73.00   75
  6  \w     94.00 173.00   1.00    7.91    --  100.00 125.00 -90.00   79
  7  \w     17.00 110.00   1.00    7.91    --  100.00 -94.00 120.00   93
  8  \w     27.00 118.00   1.00    7.91    --  100.00-125.00  90.00   91
  9  \w     17.00 110.00   1.00    7.91    --  100.00 -94.00 -60.00   93
 10  \w     74.00 173.00   1.00    7.91    --  100.00  45.00  90.00   99
 11  \w     71.00 172.00   1.00    7.91    --  100.00  61.00  30.00  101
 12  \w     28.00 129.00   1.00    7.91    --  100.00 -61.00 -30.00  101
 13  \w     27.00 118.00   1.00    7.91    --  100.00-125.00-120.00   91
 14  \w     71.00 172.00   1.00    7.91    --  100.00  61.00   0.00  101
 15  \w     24.00 133.00   1.00    7.91    --  100.00 -77.00-180.00  109
 16  \w     71.00 172.00   1.00    7.91    --  100.00  61.00 -30.00  101
 17  \w     67.00 176.00   1.00    7.91    --  100.00  77.00-120.00  109
 18  \w   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00-150.00  109
 19  \w   -115.00 -14.00   1.00    1.98    --  -42.46 -57.00  60.00  101
 20  \w   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00  30.00  109
 21  \w   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00 -60.00  109
 22  \w     23.00  98.00   1.00    1.98    --   42.46-125.00  30.00   75
 23  \w     71.00 172.00   1.00    7.91    --  100.00  61.00 120.00  101
 24  \w     67.00 169.00   1.00    7.91    --  100.00  77.00  30.00  102
 25  \w     72.00 176.00   1.00    7.91    --  100.00  30.00-180.00  104
 26  \w     71.00 172.00   1.00    7.91    --  100.00  61.00  90.00  101
 27  \w     71.00 172.00   1.00    7.91    --  100.00  61.00-180.00  101
 28  \w     67.00 176.00   1.00    7.91    --  100.00  77.00 -90.00  109
 29  \w     71.00 172.00   1.00    7.91    --  100.00  61.00-150.00  101
;
_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      -0.0312100000
_diffrn_orient_matrix_UB_12      0.1143865000
_diffrn_orient_matrix_UB_13      -0.1002182000
_diffrn_orient_matrix_UB_21      -0.0560803000
_diffrn_orient_matrix_UB_22      0.0479741000
_diffrn_orient_matrix_UB_23      0.0843475000
_diffrn_orient_matrix_UB_31      0.1517067000
_diffrn_orient_matrix_UB_32      0.0437272000
_diffrn_orient_matrix_UB_33      -0.0003430000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26350
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        70.537
_diffrn_reflns_theta_max         70.537
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.781
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.566
_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    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             647
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.5294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5009
_reflns_number_total             5431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           4_CH3CN_H2O_gard25q
_cod_original_cell_volume        1432.55(9)
_cod_original_formula_sum        'C28 H25 F3 Mn0.50 N4 O4 P S'
_cod_database_code               7249434
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C28H25N4F3O3PMnS
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.605
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.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)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              10694
_shelx_hkl_checksum              71362
_olex2_submission_original_sample_id gard25q
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.847