A five-coordinate manganese(III) complex of a salen type ligand with a positive axial anisotropy parameter D
Sova, Sergiu; Vlad, Angelica; Cazacu, Maria; Krzystek, Jurek; Bucinsky, Lukas; Breza, Martin; Darvasiova, Denisa; Rapta, P.; Cano, Joan; Telser, Joshua; Arion, Vladimir; Dalton Trans.  (2017) –; doi:10.1039/C7DT01809F

data_7043936
_publ_section_title
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 A five-coordinate manganese(III) complex of a salen type ligand with a
 positive axial anisotropy parameter D
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01809F
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H66 Mn N3 O3 S Si2, 0.4(H2 O)'
_chemical_formula_sum            'C41 H66.8 Mn N3 O3.4 S Si2'
_chemical_formula_weight         799.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-02
_audit_creation_method
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.3668(8)
_cell_length_b                   29.3668(8)
_cell_length_c                   11.7840(5)
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.6440
_cell_measurement_theta_min      1.5500
_cell_volume                     10162.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -6.00  22.20   0.30   20.00    --  -20.27 -99.00 -90.00   94
  2  \w    -36.00  50.10   0.30   20.00    --   22.46   0.00 -90.00  287
  3  \w    -25.00 -17.50   0.30   20.00    --  -20.11 -99.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0234783000
_diffrn_orient_matrix_UB_12      -0.0020484000
_diffrn_orient_matrix_UB_13      0.0132648000
_diffrn_orient_matrix_UB_21      -0.0010244000
_diffrn_orient_matrix_UB_22      -0.0205731000
_diffrn_orient_matrix_UB_23      -0.0313397000
_diffrn_orient_matrix_UB_31      0.0055959000
_diffrn_orient_matrix_UB_32      -0.0124756000
_diffrn_orient_matrix_UB_33      0.0496515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18712
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_description       prism
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1703 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8548
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0707P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                5969
_reflns_number_total             8548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01809f2.cif
_cod_data_source_block           shi_3237_av
_cod_original_cell_volume        10162.6(7)
_cod_original_formula_sum        'C41 H66.80 Mn N3 O3.40 S Si2'
_cod_database_code               7043936
_chemical_oxdiff_formula         'C30 H30 N3 O3 Si2 Mn1'
_chemical_oxdiff_usercomment     Mn_NCS
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Restrained distances
 C37-C39 \\sim C40-C37 \\sim C37-C38 \\sim C12-C11 \\sim C11-C14 \\sim C11-C13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C13)
Uanis(C40) = Uanis(C39)
4. Others
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C13X(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14X(0.5) H14D(0.5)
 H14E(0.5) H14F(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C39X(0.5) H39D(0.5)
 H39E(0.5) H39F(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C40X(0.5) H40D(0.5)
 H40E(0.5) H40F(0.5) O2W(0.15) H2WA(0.15) H2WB(0.15) O1W(0.1) H1WA(0.1)
 H1WB(0.1) O3W(0.15) H3WA(0.15) H3WB(0.15)
5.a Riding coordinates:
 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), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), 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)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.872