Manganese(ii) complex of an oxygen‒nitrogen donor Schiff base ligand showing efficient catechol oxidase activity: synthesis, spectroscopic and kinetic study
Adak, Piyali; Mondal, Antu; Chattopadhyay, Shyamal Kumar; New Journal of Chemistry 44 (2020) 3748–3754; doi:10.1039/C9NJ04591K

data_7059306
_publ_section_title
;
 Manganese(ii) complex of an oxygen--nitrogen donor Schiff base ligand
 showing efficient catechol oxidase activity: synthesis, spectroscopic and
 kinetic study
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3748
_journal_page_last               3754
_journal_paper_doi               10.1039/C9NJ04591K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(C16 H16 Mn N6 O4), H2 O0.5'
_chemical_formula_sum            'C32 H34 Mn2 N12 O8.5'
_chemical_formula_weight         832.59
_chemical_name_systematic        'Mn CRYSTAL'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-26
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-29 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3322(4)
_cell_length_b                   21.0652(9)
_cell_length_c                   16.0539(6)
_cell_measurement_reflns_used    4173
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.342
_cell_measurement_theta_min      2.536
_cell_volume                     3494.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      299.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2989
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.191
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  1.129
_exptl_absorpt_correction_T_min  1.119
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 1122 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0537P)^2^+3.7721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                2628
_reflns_number_total             2989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04591k2.cif
_cod_data_source_block           228ext_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'EMPIRICAL' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7059306.cif.

 Adding full bibliography for 7059306.cif.
;
_cod_original_formula_sum        'C32 H34 Mn2 N12 O8.50'
_cod_database_code               7059306
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.702
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Rigid body (RIGU) restrains
 O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O5(0.25) H5B(0.5) H5C(0.5)
5.a Free rotating group:
 O5(H5B,H5C)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), N2(H2), C7(H7), C4(H4), C5(H5), C13(H13), C3(H3), C2(H2A), C10(H10),
  C11(H11), C12(H12), N5(H5A)
5.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5566
_olex2_exptl_crystal_mounting_method MANUALLY
_olex2_submission_special_instructions 'No special instructions were received'