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_7249431
_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         'C30.92 H27.77 Mn N4.92 O2.08 P, C F3 O3 S'
_chemical_formula_sum            'C31.92 H27.77 F3 Mn N4.92 O5.08 P S'
_chemical_formula_weight         736.57
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-12 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.4813(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4795(2)
_cell_length_b                   12.8391(2)
_cell_length_c                   16.5133(3)
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.12
_cell_measurement_theta_min      5.87
_cell_volume                     3251.22(10)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2024)'
_computing_data_collection       'APEX-5 v2023.9-4 (Bruker, 2024)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2024)'
_computing_molecular_graphics
'ShelXle v6.4.0 Rev1506 (H\"ubschle et al, 2011)'
_computing_publication_material
;
CIFTAB-2014/2 (Sheldrick, 2008) and
FinalCif v136 (Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html)
;
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_details
'charge-integrating and photon counting pixel array'
_diffrn_detector_type            'PhotonIII C14'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture, Single Source'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_measurement_specimen_support 'MiTeGen Dual Thickness MicroMount'
_diffrn_radiation_monochromator  'HELIOS Multi-layer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            151831
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.833
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'Incoatec micro-focus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_type              'I\mS 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.949
_exptl_absorpt_correction_T_max  0.5553
_exptl_absorpt_correction_T_min  0.3676
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & 
Stalke D. (2015). <i>J. Appl. Cryst.</i> <b>48</b>, 3-10.
;
_exptl_crystal_colour            'Translucent Yellow'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1510
_exptl_crystal_recrystallization_method
'Crystals were grown by vapor diffusion of diethyl ether into acetonitrile at ambient temperature in a closed vial.'
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.049
_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     516
_refine_ls_number_reflns         7086
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0332P)^2^+2.0633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7045
_reflns_number_total             7086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           3-Mn0p92_2-Mn0p08_GARD27D
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        3251.19(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249431
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.329
_shelx_estimated_absorpt_t_max   0.622
_diffrn_measurement_ambient_temperature_device_make 'Oxford CryoStream 1000'
_shelx_res_checksum              6513
_shelx_hkl_checksum              25884