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_7708742
_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         'C24 H21 Cl Mn N7, C24 H20 Cl Mn N7, Cl'
_chemical_formula_sum            'C48 H41 Cl3 Mn2 N14'
_chemical_formula_weight         1030.18
_chemical_name_systematic        '[Mn(NTB)Cl][Mn(NTB)l]Cl'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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.r6272)
;
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.522(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3155(9)
_cell_length_b                   24.0664(16)
_cell_length_c                   17.2437(9)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      22.59
_cell_measurement_theta_min      2.21
_cell_volume                     5940.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59831
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.193
_diffrn_reflns_theta_min         2.026
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for
absorption correction
wR2(int) was 0.1148 before and 0.0615 after
correction.
;
_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    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_preparation       'MnCl2 + NTB in Ethanol at RT'
_exptl_crystal_recrystallization_method Ethanol
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0990P)^2^+0.6073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6811
_reflns_number_total             12982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01925b2.cif
_cod_data_source_block           mo_mnntbcl_3m
_cod_database_code               7708742
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C32(H32A,H32B), C40(H40A,H40B),
 C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N7(H7), N9(H9), N12(H12A), C2(H2A), C3(H3), C4(H4), C5(H5A),
 C12(H12), C13(H13), C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23),
  C26(H26), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36), C37(H37),
 C42(H42), C43(H43), C44(H44), C45(H45), C27(H27)
;
_smtbx_masks_special_details
'A solvent mask was calculated and 430 electrons were found in a volume of 1704\%A^3^ in 1 void per unit cell. This is consistent with the presence of 10[H2O] per Unit Cell which account for 400 electrons per unit cell.'
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5904
_shelx_hkl_checksum              70400
_shelx_fab_checksum              72155
_olex2_exptl_crystal_mounting_method 'In a cryoloop with mineral oil'
_olex2_submission_original_sample_id '[Mn(NTB)Cl][Mn(NTB)Cl]Cl'
_olex2_submission_special_instructions 'No special instructions were received'