Mononuclear Mn complexes featuring N,S-/N,N-donor and 1,3,5-triaza-7-phosphaadamantane ligands: synthesis and electrocatalytic properties
Kaim, Vishakha; Kaur-Ghumaan, Sandeep; New Journal of Chemistry 45 (2021) 20272–20279; doi:10.1039/D1NJ02104D

data_7061060
_publ_section_title
;
 Mononuclear Mn complexes featuring N,S-/N,N-donor and
 1,3,5-triaza-7-phosphaadamantane ligands: synthesis and electrocatalytic
 properties
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20272
_journal_page_last               20279
_journal_paper_doi               10.1039/D1NJ02104D
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H16 Mn N4 O3 P S2'
_chemical_formula_sum            'C16 H16 Mn N4 O3 P S2'
_chemical_formula_weight         462.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-28 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0708(7)
_cell_length_b                   11.9149(8)
_cell_length_c                   15.6475(11)
_cell_measurement_reflns_used    5050
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.3120
_cell_measurement_theta_min      2.3930
_cell_volume                     1877.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -25.75 154.25   1.00    2.00 -25.75   0.00  73.76    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295276000
_diffrn_orient_matrix_UB_12      -0.0523731000
_diffrn_orient_matrix_UB_13      -0.0101018000
_diffrn_orient_matrix_UB_21      -0.0254480000
_diffrn_orient_matrix_UB_22      0.0036960000
_diffrn_orient_matrix_UB_23      -0.0421560000
_diffrn_orient_matrix_UB_31      0.0586762000
_diffrn_orient_matrix_UB_32      0.0280191000
_diffrn_orient_matrix_UB_33      -0.0132734000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11170
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.668
_diffrn_reflns_theta_min         2.405
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.643
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+3.9220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3314
_reflns_number_total             3498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02104d2.cif
_cod_data_source_block           fastscan_autored
_cod_database_code               7061060
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 87.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.53
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(4)
 0.48(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C15(H15A,H15B), C12(H12A,H12B), C11(H11A,H11B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6)
;
_shelx_res_checksum              98673
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.554
_oxdiff_exptl_absorpt_empirical_full_min 0.487