Design, synthesis, structural, spectral, and redox properties and phenoxazinone synthase activity of tripodal pentacoordinate Mn(ii) complexes with impressive turnover numbers
Kumbhakar, Sadananda; Giri, Bishnubasu; Muley, Arabinda; Karumban, Kalai Selvan; Maji, Somnath; Dalton Transactions  (2021) –; doi:10.1039/D1DT01925B

data_7708743
_publ_section_title
;
 Design, synthesis, structural, spectral, and redox properties and
 phenoxazinone synthase activity of tripodal pentacoordinate Mn(ii)
 complexes with impressive turnover numbers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01925B
_journal_year                    2021
_chemical_formula_moiety         'C27 H27 Cl Mn N7, Cl'
_chemical_formula_sum            'C27 H27 Cl2 Mn N7'
_chemical_formula_weight         575.39
_chemical_name_systematic        '[Mn(Me3NTB)Cl]Cl'
_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     dual
_audit_creation_date             2021-09-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                84.817(4)
_cell_angle_beta                 64.107(4)
_cell_angle_gamma                62.525(4)
_cell_formula_units_Z            4
_cell_length_a                   14.6833(19)
_cell_length_b                   15.3453(18)
_cell_length_c                   16.604(2)
_cell_measurement_reflns_used    12255
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.3260
_cell_measurement_theta_min      2.7920
_cell_volume                     2956.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.121
_diffrn_reflns_theta_min         1.897
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_preparation       'MnCl2 + Me3NTB in MeOH at RT'
_exptl_crystal_recrystallization_method MeOH
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         13018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0909P)^2^+1.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8220
_reflns_number_total             13018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01925b2.cif
_cod_data_source_block           mo_snm_snk_mnmentbcl_1_0m
_cod_depositor_comments
;

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H54 Cl4 Mn2 N14'
_cod_original_formula_weight         1150.79
_cod_original_formula_moiety         '2(C27 H27 Cl Mn N7), 2(Cl)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2957.0(7)
_cod_database_code               7708743
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C28(H28A,H28B), C37(H37A,H37B),
 C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16),
 C24(H24), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35),
  C41(H41), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C30(H30A,H30B,
 H30C), C45(H45A,H45B,H45C), C55(H55A,H55B,H55C)
;
_smtbx_masks_special_details
'A solvent mask was calculated and 118 electrons were found in a volume of 463\%A^3^ in 2 voids per unit cell. This is consistent with the presence of 1.85[H2O], 4.05[H2O] per Unit Cell which account for 118 electrons per unit cell.'
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82007
_shelx_hkl_checksum              78266
_shelx_fab_checksum              86021
_olex2_exptl_crystal_mounting_method 'In acryoloop with mineral oil'
_olex2_submission_original_sample_id '[Mn(Me3NTB)Cl]Cl'
_olex2_submission_special_instructions 'No special instructions were received'