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_7048557
_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         'C88 H136 Mn2 N4 O10 Si4, 4(C H2 Cl2)'
_chemical_formula_sum            'C92 H144 Cl8 Mn2 N4 O10 Si4'
_chemical_formula_weight         1971.95
_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     direct
_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                73.414(5)
_cell_angle_beta                 81.359(5)
_cell_angle_gamma                72.378(5)
_cell_formula_units_Z            1
_cell_length_a                   11.8837(17)
_cell_length_b                   12.7755(19)
_cell_length_c                   18.564(3)
_cell_measurement_reflns_used    8796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.601
_cell_volume                     2568.1(7)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8962
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_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    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+13.7742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2270
_reflns_number_gt                8076
_reflns_number_total             8962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04596h2.cif
_cod_data_source_block           mo_vlar310117_p-1
_cod_depositor_comments
'Adding full bibliography for 7048556--7048558.cif.'
_cod_original_cell_volume        2568.1(6)
_cod_database_code               7048557
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7609(18)
 0.2391(18)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C16(H16A,H16B), C25(H25A,H25B), C24(H24A,
 H24B), C23(H23A,H23B), C46(H46A,H46B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C44(H44), C3(H3), C30(H30), C5(H5), C26(H26), C28(H28), C43(H43)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C38(H38A,H38B,H38C), C10(H10A,H10B,
 H10C), C40(H40A,H40B,H40C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C9(H9A,H9B,
 H9C), C34(H34A,H34B,H34C), C21(H21A,H21B,H21C), C39(H39A,H39B,H39C), C22(H22A,
 H22B,H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C20(H20A,H20B,H20C),
 C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'