A new chiral dimanganese(III) complex: synthesis, crystal structure, spectroscopic, magnetic, and catalytic properties
Andruh, Marius; Dinca, Alina Simona; Candu, Natalia; Julve, Miguel; Lloret, Francesc; Sova, Sergiu; Parvulescu, Vasile i; RSC Adv.  (2016) –; doi:10.1039/C6RA18989J

data_7226479
_publ_section_title
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 A new chiral dimanganese(III) complex: synthesis, crystal structure,
 spectroscopic, magnetic, and catalytic properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA18989J
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C74 H58 Mn2 N4 O10, 2(C3 H7 N O)'
_chemical_formula_sum            'C80 H72 Mn2 N6 O12'
_chemical_formula_weight         1419.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-09 deposited with the CCDC.
2016-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5762(2)
_cell_length_b                   24.1976(4)
_cell_length_c                   24.6149(4)
_cell_measurement_reflns_used    8506
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      26.8580
_cell_measurement_theta_min      1.6790
_cell_volume                     6895.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      200.00(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -93.00  -66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690 -178.0000  -30.0000 27

  2 omega  -38.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690   19.0000  -60.0000 26

  3 omega   21.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690   19.0000  -60.0000 35

  4 omega    2.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7471   19.0000 -150.0000 79

  5 omega  -10.00   15.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7471   77.0000  -90.0000 25

  6 omega  -39.00   36.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690   77.0000  120.0000 75
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0104286000
_diffrn_orient_matrix_UB_12      -0.0287664000
_diffrn_orient_matrix_UB_13      -0.0025394000
_diffrn_orient_matrix_UB_21      -0.0543057000
_diffrn_orient_matrix_UB_22      -0.0033229000
_diffrn_orient_matrix_UB_23      -0.0129478000
_diffrn_orient_matrix_UB_31      0.0263945000
_diffrn_orient_matrix_UB_32      0.0045334000
_diffrn_orient_matrix_UB_33      -0.0256192000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31967
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense brown'
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         12164
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+1.2590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                10617
_reflns_number_total             12164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra18989j2.cif
_cod_data_source_block           shi_1905_maan
_cod_original_cell_volume        6895.1(2)
_cod_database_code               7226479
_chemical_oxdiff_formula         'C50 H50 N12 O6 Mn1 Fe1'
_chemical_oxdiff_usercomment     '_519'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C78X \\sim N6-C77 \\sim N6-C77X \\sim N6-C78
 with sigma of 0.01
 N6-C76X \\sim N6-C76
 with sigma of 0.01
 O12-C76 \\sim O12-C76X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C78) = Uiso(C77X) = Uiso(C77) = Uiso(C78X)
4. Others
 Fixed Sof: C76(0.5) H76(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C78(0.5)
 H78A(0.5) H78B(0.5) H78C(0.5) C76X(0.5) H76X(0.5) C77X(0.5) H77D(0.5)
 H77E(0.5) H77F(0.5) C78X(0.5) H78D(0.5) H78E(0.5) H78F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41),
 C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C57(H57),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C67(H67),
 C68(H68), C69(H69), C76(H76), C76X(H76X), C73(H73)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C72(H72A,H72B,
 H72C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C77X(H77D,H77E,H77F), C78X(H78D,H78E,H78F), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C)
;
_olex2_submission_special_instructions 'No special instructions were received'