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_7043179
_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         'C36 H36 Cu3 Mn N4 O8, 4(H2 O), B F4'
_chemical_formula_sum            'C36 H44 B Cu3 F4 Mn N4 O12'
_chemical_formula_weight         1057.12
_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
;
2017-05-09 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.479(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8093(9)
_cell_length_b                   13.6009(7)
_cell_length_c                   19.1235(10)
_cell_measurement_reflns_used    6535
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.0860
_cell_measurement_theta_min      3.1560
_cell_volume                     4364.0(4)
_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      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details
;
  1 omega  -30.00   71.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438  -92.0000   74.0000 101

  2 omega   59.00  111.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438  179.0000  -90.0000 52

  3 omega   37.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438  -92.0000 -105.0000 26

  4 omega   44.00   70.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438  179.0000 -150.0000 26

  5 omega   -1.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438   77.0000    0.0000 66

  6 omega   18.00  103.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438   77.0000 -120.0000 85

  7 omega  -36.00  103.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438    0.0000   60.0000 139

  8 omega   -2.00   41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7438   77.0000  120.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0286906000
_diffrn_orient_matrix_UB_12      0.0249977000
_diffrn_orient_matrix_UB_13      -0.0221443000
_diffrn_orient_matrix_UB_21      -0.0062963000
_diffrn_orient_matrix_UB_22      0.0340143000
_diffrn_orient_matrix_UB_23      0.0272408000
_diffrn_orient_matrix_UB_31      0.0304093000
_diffrn_orient_matrix_UB_32      0.0306333000
_diffrn_orient_matrix_UB_33      -0.0121527000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51481
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.711
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24317
_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    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL 4 in P2(1)/n
CELL   16.8093   13.6009   19.1235     90.00     93.48     90.00
SPGR P21/n
C101 0.902 0.968 0.482 !       1.41 eA-3
Q102 0.973 0.945 0.031 !       1.02 eA-3
Q103 0.989 0.149 0.485 !       1.01 eA-3
Q104 0.437 0.405 0.408 !       1.00 eA-3
Q105 0.041 0.441 0.449 !       0.99 eA-3
C106 0.611 0.510 0.012 !       0.99 eA-3
Q107 0.173 0.642 0.404 !       0.94 eA-3
Q108 0.039 0.126 0.497 !       0.93 eA-3
Q109 0.255 0.808 0.436 !       0.92 eA-3
Q110 0.141 0.619 0.487 !       0.91 eA-3
Q111 0.940 0.140 0.495 !       0.86 eA-3
Q112 0.604 0.481 0.067 !       0.85 eA-3
Q113 0.645 0.750 0.203 !       0.85 eA-3
Q114 0.627 0.626 0.451 !       0.83 eA-3
Q115 0.125 0.593 0.437 !       0.79 eA-3
C116 0.999 0.897 0.481 !       0.78 eA-3
Q117 0.201 0.857 0.075 !       0.78 eA-3
Q118 0.499 0.235 0.018 !       0.78 eA-3
Q119 0.484 0.470 0.407 !       0.77 eA-3
C120 0.983 0.871 0.467 !       0.75 eA-3
Q121 0.750 0.076 0.186 !       0.75 eA-3
Q122 0.035 0.892 0.452 !       0.72 eA-3
Q123 0.059 0.078 0.455 !       0.71 eA-3
Q124 0.612 0.233 0.456 !       0.71 eA-3
Q125 0.655 0.454 0.406 !       0.71 eA-3
C126 0.483 0.654 0.970 !       0.71 eA-3
Q127 0.060 0.998 0.063 !       0.70 eA-3
Q128 0.676 0.734 0.079 !       0.70 eA-3
Q129 0.874 0.739 0.331 !       0.69 eA-3
Q130 0.949 0.096 0.112 !       0.69 eA-3
Q131 0.277 0.839 0.043 !       0.69 eA-3
Q132 0.031 1.002 0.484 !       0.69 eA-3
Q133 0.562 0.721 0.343 !       0.67 eA-3
Q134 0.474 0.643 0.049 !       0.67 eA-3
Q135 0.311 0.020 0.123 !       0.67 eA-3
Q136 0.611 0.186 0.018 !       0.67 eA-3
Q137 0.409 0.393 0.456 !       0.66 eA-3
Q138 0.278 0.468 0.374 !       0.66 eA-3
Q139 0.082 1.010 0.486 !       0.66 eA-3
Q140 0.796 0.804 0.077 !       0.66 eA-3
Q141 0.465 0.184 0.030 !       0.66 eA-3
Q142 0.124 0.870 0.091 !       0.66 eA-3
Q143 0.306 0.452 0.276 !       0.65 eA-3
Q144 0.420 0.984 0.034 !       0.65 eA-3
Q145 0.849 0.871 0.439 !       0.65 eA-3
Q146 0.393 0.766 0.409 !       0.65 eA-3
Q147 0.828 0.674 0.328 !       0.65 eA-3
Q148 0.947 0.941 0.485 !       0.64 eA-3
Q149 0.794 0.782 0.295 !       0.64 eA-3
Q150 0.935 0.316 0.487 !       0.64 eA-3
Q151 0.970 0.145 0.441 !       0.64 eA-3
Q152 0.951 0.171 0.470 !       0.64 eA-3
Q153 0.218 0.655 0.294 !       0.63 eA-3
C154 0.940 0.845 0.437 !       0.63 eA-3
Q155 0.869 0.254 0.405 !       0.63 eA-3
Q156 0.546 0.834 0.134 !       0.63 eA-3
Q157 0.127 0.079 0.017 !       0.63 eA-3
Q158 0.956 0.406 0.435 !       0.63 eA-3
Q159 0.105 0.355 0.425 !       0.63 eA-3
Q160 0.179 0.593 0.444 !       0.63 eA-3
Q161 0.499 0.872 0.032 !       0.63 eA-3
Q162 0.551 0.058 0.013 !       0.63 eA-3
Q163 0.576 0.655 0.044 !       0.62 eA-3
Q164 0.996 0.176 0.407 !       0.62 eA-3
Q165 0.840 0.094 0.422 !       0.62 eA-3
Q166 0.231 0.097 0.487 !       0.62 eA-3
Q167 0.474 0.422 0.325 !       0.62 eA-3
Q168 0.560 0.203 0.013 !       0.61 eA-3
Q169 0.670 0.108 0.078 !       0.61 eA-3
Q170 0.856 0.059 0.487 !       0.61 eA-3
C171 0.658 0.093 0.438 !       0.61 eA-3
Q172 0.451 0.627 0.423 !       0.61 eA-3
Q173 0.022 0.329 0.440 !       0.60 eA-3
Q174 0.700 0.357 0.447 !       0.60 eA-3
Q175 0.939 0.215 0.438 !       0.60 eA-3
Q176 0.021 0.478 0.483 !       0.60 eA-3
Q177 0.283 0.488 0.081 !       0.60 eA-3
Q178 0.233 0.028 0.284 !       0.59 eA-3
Q179 0.815 0.174 0.358 !       0.59 eA-3
Q180 0.924 0.154 0.131 !       0.59 eA-3
Q181 0.122 0.127 0.157 !       0.59 eA-3
Q182 0.730 0.718 0.407 !       0.59 eA-3
Q183 0.984 0.924 0.452 !       0.59 eA-3
Q184 0.972 0.936 0.402 !       0.59 eA-3
Q185 0.933 0.947 0.453 !       0.59 eA-3
C186 0.918 0.911 0.472 !       0.59 eA-3
Q187 0.307 1.001 0.345 !       0.59 eA-3
Q188 0.126 0.358 0.061 !       0.59 eA-3
Q189 0.957 0.203 0.017 !       0.59 eA-3
Q190 0.730 0.089 0.264 !       0.58 eA-3
Q191 0.756 0.157 0.213 !       0.58 eA-3
Q192 0.530 0.088 0.062 !       0.58 eA-3
Q193 0.300 0.294 0.504 !       0.58 eA-3
Q194 0.717 0.080 0.325 !       0.58 eA-3
Q195 0.127 0.661 0.417 !       0.58 eA-3
Q196 0.254 0.346 0.375 !       0.58 eA-3
Q197 0.940 0.730 0.155 !       0.58 eA-3
Q198 0.855 0.655 0.156 !       0.58 eA-3
Q199 0.358 0.533 0.407 !       0.58 eA-3
;
_refine_diff_density_max         1.469
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         14779
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5567
_reflns_number_total             14779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00957g2.cif
_cod_data_source_block           4_sq
_cod_database_code               7043179
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.614
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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. Restrained distances
 OW1-HW1A = OW1-HW1B
 0.85 with sigma of 0.005
 OW3-HW3A
 0.85 with sigma of 0.001
 OW3-HW3B
 0.85 with sigma of 0.001
 HW3A-HW3B
 1.5 with sigma of 0.005
 HW1A-O3
 1.95 with sigma of 0.005
 HW3A-O5
 1.85 with sigma of 0.005
 OW4A-HW3B_$1
 2.42 with sigma of 0.005
 HW4A-HW4B
 1.4 with sigma of 0.005
 OW4A-HW4A = OW4A-HW4B
 0.85 with sigma of 0.001
 HW4A-O7
 1.95 with sigma of 0.005
 HW1B-F1_$2
 2.15 with sigma of 0.005
 OW2A-HW2A = OW2A-HW2B
 0.85 with sigma of 0.005
 HW2A-HW2B
 1.4 with sigma of 0.005
 HW2A-O1
 1.95 with sigma of 0.005
 B1-F1 \\sim B1-F2A \\sim B1-F3A \\sim B1-F4A \\sim B1-F2B \\sim B1-F3B \\sim
B1-F4B
 with sigma of 0.01
 F1-F4A \\sim F2A-F3A \\sim F1-F2A \\sim F3A-F4A \\sim F1-F3A \\sim F2A-F4A
 with sigma of 0.02
 F1-F2B \\sim F3B-F4B \\sim F1-F3B \\sim F1-F4B \\sim F2B-F3B \\sim F2B-F4B
 with sigma of 0.02
3. Rigid bond restraints
 F1, F2A, F2B, F3A, F3B, F4A, F4B, B1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim F4A \\sim F4B \\sim B1: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
OW4A \\sim OW4B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F4B) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(OW4B) \\sim Ueq, Uanis(OW4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(OW1) \\sim Ueq, Uanis(OW3) \\sim Ueq, Uanis(OW2A) \\sim Ueq, Uanis(OW4A)
\\sim Ueq, Uanis(OW4B) \\sim Ueq: with sigma of 0.1 and sigma for terminal
atoms of 0.2
5. Others
 Fixed Sof: F2A(0.55) F2B(0.45) F3A(0.55) F3B(0.45) F4A(0.55) F4B(0.45)
 OW4A(0.6) HW4A(0.6) HW4B(0.6) OW4B(0.4) HW4C(0.4) HW4D(0.4)
6.a Riding coordinates:
 OW2A(HW2A,HW2B), OW4A(HW4A,HW4B), OW4B(HW4C,HW4D), OW3(HW3A,HW3B), OW1(HW1A,
 HW1B)
6.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)
6.c 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'