Expanding manganese(IV) aqueous chemistry: unusually stable water-soluble hexahydrazide clathrochelate complexes.
Shylin, Sergii I.; Pogrebetsky, James L.; Husak, Alina O.; Bykov, Dmytro; Mokhir, Andriy; Hampel, Frank; Shova, Sergiu; Ozarowski, Andrew; Gumienna-Kontecka, Elzbieta; Fritsky, Igor O.; Chemical communications (Cambridge, England) 57 (2021) 11060–11063; doi:10.1039/d1cc04870h

data_7129015
_publ_section_title
;
 Expanding manganese(IV) aqueous chemistry: unusually stable water-soluble
 hexahydrazide clathrochelate complexes.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11060
_journal_page_last               11063
_journal_paper_doi               10.1039/d1cc04870h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'2(C24 H20 As), C12 H12 Mn N12 O6, 13.5(H2 O)'
_chemical_formula_sum            'C60 H79 As2 Mn N12 O19.5'
_chemical_formula_weight         1485.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-11 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0876(3)
_cell_length_b                   21.1132(2)
_cell_length_c                   29.7036(3)
_cell_measurement_reflns_used    17469
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      61.5530
_cell_measurement_theta_min      2.9740
_cell_volume                     13224.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6144
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
  1 omega  -19.00   70.00   1.0000    1.5300
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -120.0000 89

  2 omega   63.00  152.00   1.0000    6.1150
omega____ theta____ kappa____ phi______ frames
    -       82.5931   45.0000   30.0000 89

  3 omega   95.00  156.00   1.0000    6.1150
omega____ theta____ kappa____ phi______ frames
    -       82.5931  125.0000 -120.0000 61

  4 omega   65.00  154.00   1.0000    6.1150
omega____ theta____ kappa____ phi______ frames
    -       82.5931   77.0000 -180.0000 89

  5 omega   10.00   98.00   1.0000    6.1150
omega____ theta____ kappa____ phi______ frames
    -       82.5931  -45.0000  120.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0299257000
_diffrn_orient_matrix_UB_12      0.0426437000
_diffrn_orient_matrix_UB_13      -0.0363330000
_diffrn_orient_matrix_UB_21      0.0666401000
_diffrn_orient_matrix_UB_22      0.0174686000
_diffrn_orient_matrix_UB_23      -0.0173030000
_diffrn_orient_matrix_UB_31      -0.0020255000
_diffrn_orient_matrix_UB_32      -0.0565056000
_diffrn_orient_matrix_UB_33      -0.0327502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.795
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32460
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.614
_diffrn_reflns_theta_min         2.975
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             6160
_exptl_crystal_recrystallization_method 'crystallized from H2O'
_exptl_crystal_size_max          0.1428
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.1202
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0760P)^2^+10.9517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8448
_reflns_number_total             9514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04870h2.cif
_cod_data_source_block           anm01
_cod_depositor_comments
'Adding full bibliography for 7129015--7129016.cif.'
_cod_original_formula_sum        'C60 H79 As2 Mn N12 O19.50'
_cod_database_code               7129015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C32 H28 N12 O6 As Mn'
_reflns_odcompleteness_completeness 79.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H,H) groups
2. Others
 Fixed Sof: O301(0.5) H30K(0.5) H30L(0.5)
3.a Free rotating group:
 O312(H31A,H31B), O313(H31C,H31D), O303(H30A,H30B), O309(H30C,H30D), O307(H30E,
 H30F), O302(H30G,H30H), O310(H31E,H31F), O308(H30I,H30J), O301(H30K,H30L),
 O306(H30M,H30N), O311(H31G,H31H), O304(H30O,H30P), O314(H31I,H31J), O305(H30Q,
 H30R)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C122(H122), C123(H123),
 C124(H124), C125(H125), C126(H126), C132(H132), C133(H133), C134(H134),
 C135(H135), C136(H136), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206), C213(H213), C214(H214), C215(H215), C216(H216), C217(H217),
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C232(H232),
 C233(H233), C234(H234), C235(H235), C236(H236)
;
_olex2_date_sample_data_collection 2015-07-20
_olex2_date_sample_submission    1436911200
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_olex2_submission_special_instructions 'No special instructions were received'