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_7048558
_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         'C84 H134 Mn2 N4 O10 Si4, 6(C H2 Cl2)'
_chemical_formula_sum            'C90 H146 Cl12 Mn2 N4 O10 Si4'
_chemical_formula_weight         2091.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                67.7592(16)
_cell_angle_beta                 66.1603(17)
_cell_angle_gamma                79.2085(17)
_cell_formula_units_Z            1
_cell_length_a                   13.7007(7)
_cell_length_b                   14.7166(7)
_cell_length_c                   15.9617(8)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.939
_cell_measurement_theta_min      2.571
_cell_volume                     2722.5(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61020
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1376 before and 0.0405 after correction. The Ratio of minimum to maximum transmission is 0.8531. 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    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.523
_exptl_crystal_size_min          0.485
_refine_diff_density_max         1.036
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         15855
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1007P)^2^+1.5548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                11987
_reflns_number_total             15855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04596h2.cif
_cod_data_source_block           mo_vlar03022017_p-1
_cod_depositor_comments
'Adding full bibliography for 7048556--7048558.cif.'
_cod_database_code               7048558
_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
2. Restrained distances
 Cl4-C44 \\sim Cl1A-C58 \\sim Cl3-C58 \\sim Cl3-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C44) = Uanis(C58)
4. Others
 Fixed Sof: Cl1A(0.75) Cl4(0.25) C44(0.25) H44A(0.25) H44B(0.25) C58(0.75)
 H58A(0.75) H58B(0.75) Cl5(0.25) Cl6(0.25) C45(0.25) H45A(0.25) H45B(0.25)
 Cl7(0.75) Cl8(0.75) C46(0.75) H46A(0.75) H46B(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C44(H44A,H44B), C58(H58A,H58B), C45(H45A,H45B),
 C43(H43A,H43B), C46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C26(H26), C28(H28), C30(H30), C42(H42)
5.c 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), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'