Details make the difference: a family of tetranuclear CuIIMnIII complexes with cube-like and double open cube-like cores
Stetsiuk, Oleh; Nesterova, Oksana V.; Kokozay, Vladimir N.; Domasevitch, Kostiantyn V.; Omelchenko, Iryna V.; Shishkin, Oleg V.; Vranovičová, Beata; Boča, Roman; Pombeiro, Armando J. L.; Petrusenko, Svitlana R.; Dalton Trans.  (2017) –; doi:10.1039/C7DT00957G

data_7043177
_publ_section_title
;
 Details make the difference: a family of tetranuclear CuIIMnIII complexes
 with cube-like and double open cube-like cores
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00957G
_journal_year                    2017
_chemical_formula_moiety         'Br, C37 H44 Cu3 Mn N4 O11, H2 O'
_chemical_formula_sum            'C37 H46 Br Cu3 Mn N4 O12'
_chemical_formula_weight         1064.25
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.001(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9628(14)
_cell_length_b                   13.0651(9)
_cell_length_c                   19.7336(14)
_cell_measurement_reflns_used    2771
_cell_measurement_temperature    105.0
_cell_measurement_theta_max      24.7370
_cell_measurement_theta_min      3.2220
_cell_volume                     4605.8(6)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies, 2014'
_computing_data_collection       'CrysAlisPro, Agilent Technologies, 2014'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies, 2014'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
  1 omega   10.00   81.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0249   77.0000    0.0000 71

  2 omega   49.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0249   77.0000 -150.0000 38

  3 omega   48.00   76.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0249   77.0000  -90.0000 28

  4 omega    0.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0249   77.0000   90.0000 93

  5 omega -103.00  -32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7749  179.0000 -180.0000 71

  6 omega -103.00  -96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7749  179.0000    0.0000 7
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0378928000
_diffrn_orient_matrix_UB_12      -0.0103674000
_diffrn_orient_matrix_UB_13      -0.0045721000
_diffrn_orient_matrix_UB_21      -0.0062909000
_diffrn_orient_matrix_UB_22      0.0172069000
_diffrn_orient_matrix_UB_23      -0.0342304000
_diffrn_orient_matrix_UB_31      0.0099679000
_diffrn_orient_matrix_UB_32      0.0504394000
_diffrn_orient_matrix_UB_33      0.0107057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_unetI/netI     0.1903
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23351
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, 2014 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL koko434 in P2(1)/n
CELL   17.9628   13.0651   19.7336     90.00     96.00     90.00
SPGR P21/n
C101 0.092 0.614 0.378 !       5.95 eA-3
C102 0.600 0.974 0.033 !       2.91 eA-3
C103 0.875 0.499 0.464 !       2.47 eA-3
C104 0.792 0.524 0.419 !       2.27 eA-3
Q105 0.265 0.451 0.109 !       1.70 eA-3
C106 0.766 0.078 0.108 !       1.69 eA-3
Q107 0.932 0.457 0.417 !       1.68 eA-3
Q108 1.003 0.318 0.486 !       1.61 eA-3
Q109 0.024 0.380 0.483 !       1.44 eA-3
Q110 0.028 0.754 0.420 !       1.44 eA-3
Q111 0.518 0.969 0.261 !       1.43 eA-3
C112 0.377 0.081 0.063 !       1.42 eA-3
Q113 0.345 0.148 0.373 !       1.37 eA-3
Q114 0.808 0.370 0.075 !       1.36 eA-3
C115 0.764 0.580 0.384 !       1.32 eA-3
Q116 0.046 0.446 0.191 !       1.31 eA-3
Q117 0.080 0.725 0.359 !       1.28 eA-3
Q118 0.734 0.783 0.488 !       1.24 eA-3
Q119 0.450 0.064 0.171 !       1.23 eA-3
C120 0.407 0.133 0.065 !       1.21 eA-3
Q121 0.035 0.020 0.355 !       1.18 eA-3
Q122 0.593 0.923 0.372 !       1.16 eA-3
Q123 0.255 0.332 0.097 !       1.13 eA-3
Q124 0.800 0.691 0.458 !       1.13 eA-3
Q125 0.376 0.689 0.156 !       1.12 eA-3
Q126 0.799 0.482 0.073 !       1.12 eA-3
Q127 0.780 0.453 0.035 !       1.11 eA-3
Q128 0.220 0.445 0.030 !       1.11 eA-3
C129 0.573 0.052-0.003 !       1.11 eA-3
Q130 0.345 0.669 0.042 !       1.11 eA-3
Q131 0.747 0.040 0.143 !       1.10 eA-3
C132 0.824 0.523 0.469 !       1.09 eA-3
Q133 0.111 0.237 0.498 !       1.08 eA-3
Q134 0.136 0.149 0.392 !       1.08 eA-3
Q135 0.389 0.562 0.098 !       1.05 eA-3
Q136 0.139 0.364 0.488 !       1.05 eA-3
C137 0.982 0.423 0.492 !       1.05 eA-3
Q138 0.644 0.391 0.404 !       1.04 eA-3
Q139 0.221 0.813 0.363 !       1.04 eA-3
Q140 0.298 0.750 0.045 !       1.03 eA-3
Q141 0.762 0.156 0.125 !       1.03 eA-3
Q142 1.002 0.560 0.451 !       1.02 eA-3
Q143 0.308 0.376 0.091 !       1.02 eA-3
Q144 0.503 0.156 0.281 !       1.02 eA-3
Q145 0.721 0.688 0.855 !       1.02 eA-3
Q146 0.599 0.157 0.047 !       1.01 eA-3
Q147 0.188 0.310 0.283 !       1.01 eA-3
Q148 0.535 0.013 0.279 !       1.01 eA-3
Q149 1.001 0.619 0.489 !       1.01 eA-3
C150 0.824 0.583 0.404 !       1.01 eA-3
Q151 0.763 0.517 0.158 !       1.00 eA-3
Q152 0.686 0.577 0.387 !       1.00 eA-3
Q153 0.626 0.516 0.325 !       1.00 eA-3
Q154 0.235 0.343 0.047 !       1.00 eA-3
Q155 0.996 0.439 0.451 !       0.99 eA-3
Q156 0.385 0.609 0.125 !       0.99 eA-3
Q157 0.576 0.623 0.470 !       0.99 eA-3
Q158 0.438 0.344 0.246 !       0.98 eA-3
C159 0.340 0.979 0.015 !       0.98 eA-3
Q160 0.239 0.966 0.467 !       0.98 eA-3
Q161 0.702 0.419 0.390 !       0.98 eA-3
Q162 0.156 0.232 0.311 !       0.98 eA-3
Q163 0.168 0.035 0.432 !       0.97 eA-3
Q164 0.608 0.047 0.435 !       0.97 eA-3
Q165 0.119 0.691 0.358 !       0.97 eA-3
Q166 0.029 0.926 0.050 !       0.96 eA-3
Q167 0.073 0.910 0.297 !       0.96 eA-3
Q168 0.301 0.074 0.378 !       0.95 eA-3
Q169 0.109 0.018 0.171 !       0.94 eA-3
Q170 0.307 0.610 0.032 !       0.94 eA-3
Q171 0.141 0.656 0.068 !       0.94 eA-3
Q172 0.495 0.911 0.235 !       0.94 eA-3
Q173 0.812 0.626 0.102 !       0.94 eA-3
Q174 0.417 0.621 0.168 !       0.93 eA-3
Q175 0.376 0.524 0.266 !       0.93 eA-3
Q176 0.093 0.532 0.408 !       0.92 eA-3
C177 0.061 0.619 0.449 !       0.92 eA-3
Q178 0.422 0.375 0.358 !       0.92 eA-3
Q179 0.814 1.001 0.408 !       0.92 eA-3
Q180 0.760 0.045 0.394 !       0.92 eA-3
Q181 0.094 0.267 0.469 !       0.92 eA-3
Q182 0.406 0.331 0.109 !       0.92 eA-3
Q183 0.755 0.373 0.030 !       0.91 eA-3
Q184 0.549 0.239 0.002 !       0.91 eA-3
Q185 0.627 0.139 0.219 !       0.91 eA-3
Q186 0.593 0.588 0.124 !       0.91 eA-3
Q187 0.596 0.652 0.407 !       0.91 eA-3
Q188 0.380 0.688 0.080 !       0.91 eA-3
Q189 0.827 0.440 0.078 !       0.91 eA-3
Q190 0.303 1.007 0.028 !       0.91 eA-3
Q191 0.189 0.929 0.370 !       0.90 eA-3
Q192 0.464 0.409 0.343 !       0.90 eA-3
Q193 0.829 0.548 0.127 !       0.90 eA-3
Q194 0.423 0.844 0.011 !       0.90 eA-3
Q195 0.416 0.581 0.062 !       0.90 eA-3
Q196 0.171 0.377 0.317 !       0.90 eA-3
Q197 0.177 0.356 0.372 !       0.90 eA-3
Q198 0.310 0.126 0.312 !       0.89 eA-3
C199 0.688 0.050 0.124 !       0.89 eA-3
;
_refine_diff_density_max         1.366
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10477
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.2190
_refine_ls_R_factor_gt           0.1023
_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^)+(0.1347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2433
_refine_ls_wR_factor_ref         0.3183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4162
_reflns_number_total             10477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00957g2.cif
_cod_data_source_block           koko434_sq
_cod_database_code               7043177
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.628
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1S-C1SA \\sim O1S-C1SB
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1SA \\sim C1SB: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
O4SA \\sim O4SB: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C1SB) \\sim Ueq, Uanis(C1SA) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Fixed Sof: Br1A(0.68) O4SA(0.6) H4SA(0.6) H4SB(0.6) O4SB(0.4) H4SC(0.4)
 H4SD(0.4) C1SA(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C1SB(0.5) H1SD(0.5)
 H1SE(0.5) H1SF(0.5) Br1B(0.32)
5.a Riding coordinates:
 O1S(H1S), O2S(H2SA,H2SB), O3S(H3SA,H3SB), O4SA(H4SA,H4SB), O4SB(H4SC,H4SD)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B),
 C27(H27A,H27B), C35(H35A,H35B), C36(H36A,H36B)
5.c Me refined with riding coordinates:
 C1SA(H1SA,H1SB,H1SC), C1SB(H1SD,H1SE,H1SF)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'