Dinuclear manganese(iii) complexes with bioinspired coordination and variable linkers showing weak exchange effects: a synthetic, structural, spectroscopic and computation study.
Shova, Sergiu; Vlad, Angelica; Cazacu, Maria; Krzystek, J.; Ozarowski, Andrew; Malček, Michal; Bucinsky, Lukas; Rapta, Peter; Cano, Joan; Telser, Joshua; Arion, Vladimir B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5909–5922; doi:10.1039/c8dt04596h

data_7048556
_publ_section_title
;
 Dinuclear manganese(iii) complexes with bioinspired coordination and
 variable linkers showing weak exchange effects: a synthetic, structural,
 spectroscopic and computation study.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5909
_journal_page_last               5922
_journal_paper_doi               10.1039/c8dt04596h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C94 H140 Mn2 N4 O10 Si4, 5.5(H2 O)'
_chemical_formula_sum            'C94 H151 Mn2 N4 O15.5 Si4'
_chemical_formula_weight         1807.43
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.126(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.790(2)
_cell_length_b                   14.221(2)
_cell_length_c                   23.958(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.28
_cell_volume                     5168.1(12)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64669
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1019 before and 0.0375 after correction. The Ratio of minimum to maximum transmission is 0.8870. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.877
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.086
_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     567
_refine_ls_number_reflns         9090
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+12.5516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2170
_reflns_number_gt                7227
_reflns_number_total             9090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04596h2.cif
_cod_data_source_block           mo_vlar300117_p21c
_cod_depositor_comments
'Adding full bibliography for 7048556--7048558.cif.'
_cod_original_cell_volume        5168.3(13)
_cod_original_formula_sum        'C94 H151 Mn2 N4 O15.50 Si4'
_cod_database_code               7048556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C42X-C41X \\sim C41-C42
 with sigma of 0.01
 O5-C41 \\sim O5X-C41X
 with sigma of 0.01
 O4-C41 \\sim O4X-C41X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3X) = Uanis(O3)
Uanis(Si1) = Uanis(Si1X)
Uiso(C20X) = Uiso(C19) = Uiso(C19X) = Uiso(C20)
4. Others
 Sof(Si1X)=Sof(O3X)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20X)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(Si1)=Sof(O3)=Sof(C19X)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=FVAR(1)
 Fixed Sof: Si2(0.5) Si2X(0.5) O4(0.5) O4X(0.5) O5(0.5) O5X(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) H18D(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C21X(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C22X(0.5)
 H22D(0.5) H22E(0.5) H22F(0.5) H23C(0.5) H23D(0.5) H23A(0.5) H23B(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5) C34X(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C35(0.5)
 H35A(0.5) H35B(0.5) H35C(0.5) C35X(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) H36C(0.5) C36X(0.5) H36D(0.5) H36E(0.5) H36F(0.5) C41(0.5)
 C41X(0.5) C44(0.5) H44(0.5) C45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5)
 C42(0.5) C43(0.5) H43(0.5) C47X(0.5) H47X(0.5) C42X(0.5) C43X(0.5) H43X(0.5)
 C44X(0.5) H44X(0.5) C45X(0.5) C46X(0.5) H46X(0.5) O4W(0.25) H4WA(0.25)
 H4WB(0.25) O6W(0.25) H6WA(0.25) H6WB(0.25) O1W(0.25) H1WA(0.25) H1WB(0.25)
 O5W(0.25) H5WA(0.25) H5WB(0.25) O2W(0.75) H2WA(0.75) H2WB(0.75) O3W(0.75)
 H3WA(0.75) H3WB(0.75) O7W(0.25) H7WA(0.25) H7WB(0.25)
5.a Riding coordinates:
 C19(H19A,H19B,H19C), O4W(H4WA,H4WB), O6W(H6WA,H6WB), O1W(H1WA,H1WB), O5W(H5WA,
 H5WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O7W(H7WA,H7WB)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D), C23(H23C,
 H23D), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C26(H26), C28(H28), C30(H30), C44(H44), C46(H46),
 C47(H47), C43(H43), C47X(H47X), C43X(H43X), C44X(H44X), C46X(H46X)
5.d Fitted hexagon refined as free rotating group:
 C44(C45,C46,C47,C42,C43), C47X(C42X,C43X,C44X,C45X,C46X)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19X(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20X(H20D,H20E,H20F), C21(H21A,H21B,H21C), C21X(H21D,H21E,H21F),
 C22(H22A,H22B,H22C), C22X(H22D,H22E,H22F), C34(H34A,H34B,H34C), C34X(H34D,H34E,
 H34F), C35(H35A,H35B,H35C), C35X(H35D,H35E,H35F), C36(H36A,H36B,H36C),
 C36X(H36D,H36E,H36F), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'