Ligand-directed synthesis of {MnIII5} twisted bow-ties
Murrie, Mark; Heras Ojea, Maria Jose; Hay, Moya; Cioncoloni, Giacomo; Craig, Gavin A.; Wilson, Claire; Shiga, Takuya; Oshio, Hiroki; Symes, Mark D.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02430D

data_7043864
_publ_section_title
;
 Ligand-directed synthesis of {MnIII5} twisted bow-ties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02430D
_journal_year                    2017
_chemical_formula_moiety
'C44 H40 Mn5 N20 O14, C6.7 H15 N ,2 (C H4 O), C2 H3 N'
_chemical_formula_sum            'C54 H67 Mn5 N22 O16'
_chemical_formula_weight         1554.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-09
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.877(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0222(3)
_cell_length_b                   12.0473(4)
_cell_length_c                   49.8716(12)
_cell_measurement_reflns_used    17612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1680
_cell_measurement_theta_min      2.3620
_cell_volume                     7222.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -113.00  21.00   0.50   60.00    --  -23.00 -54.00  60.00  268
  2  \w   -101.50  13.00   0.50   60.00    --  -23.00 -18.00  90.00  229
  3  \w    -18.00  26.00   0.50   60.00    --  -23.00  54.00   0.00   88
  4  \w    -63.00 -43.00   0.50   60.00    --  -23.00  36.00 -90.00   40
  5  \w   -113.00  15.00   0.50   60.00    --  -23.00 -36.00 120.00  256
  6  \w    -85.50 -16.50   0.50   60.00    --  -23.00 -72.00  60.00  138
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130291000
_diffrn_orient_matrix_UB_12      -0.0288852000
_diffrn_orient_matrix_UB_13      -0.0120465000
_diffrn_orient_matrix_UB_21      -0.0571648000
_diffrn_orient_matrix_UB_22      0.0006218000
_diffrn_orient_matrix_UB_23      0.0033000000
_diffrn_orient_matrix_UB_31      -0.0065653000
_diffrn_orient_matrix_UB_32      0.0513004000
_diffrn_orient_matrix_UB_33      -0.0068139000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            54397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68771
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         12756
_refine_ls_number_restraints     988
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0594P)^2^+50.0384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              59
_reflns_limit_l_min              -12
_reflns_number_gt                10943
_reflns_number_total             12764
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02430d2.cif
_cod_data_source_block           mn5L2
_cod_database_code               7043864
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C2S2-C2S1
 1.54 with sigma of 0.02
 O2S-C2S
 1.43 with sigma of 0.02
 C2SD-O2SD
 1.43 with sigma of 0.02
 N1SB-C1SB = N1SB-C1SA = N1SA-C1SA = N1SA-C1SC = N1SA-C1SD = N1SB-C1SC
 1.47 with sigma of 0.02
 C2SB-C1SB = C2SA-C1SA = C2SC-C1SC = C2SD-C1SD
 1.51 with sigma of 0.02
 C1SC-C1SB \\sim C1SC-C1SA \\sim C1SC-C1SD \\sim C1SD-C1SA
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1SA(0.8) H1SB(0.8) H1SC(0.8) H1SD(0.8) H1SE(0.2) H1SF(0.2)
 O2SD(0.7) C2SD(0.9) N1SB(0.8) H1SG(0.8) C1SB(0.8) H1SH(0.8) H1SI(0.8)
 C2SB(0.8) H2SG(0.8) H2SH(0.8) H2SI(0.8) N1SA(0.2) H1SJ(0.2) C2S(0.3) O2S(0.3)
 C1SD(0.2) H1SK(0.2) H1SL(0.2)
5.a Rotating group:
 N4B(H4BA,H4BB), N4C(H4CA,H4CB), N4D(H4DA,H4DB)
5.b Ternary CH refined with riding coordinates:
 N1SB(H1SG), N1SA(H1SJ)
5.c Secondary CH2 refined with riding coordinates:
 C1SA(H1SA,H1SB), C1SC(H1SC,H1SD), C1SC(H1SE,H1SF), C1SB(H1SH,H1SI), C1SD(H1SK,
 H1SL)
5.d Me refined with riding coordinates:
 C2SA(H2SA,H2SB,H2SC), C2SC(H2SD,H2SE,H2SF), C2SB(H2SG,H2SH,H2SI)
5.e Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C3C(H3C), C3D(H3D), C6A(H6AA), C6B(H6BA), C6C(H6CA),
 C6D(H6D), C7A(H7A), C7B(H7B), C7C(H7C), C7D(H7D), C8A(H8AA), C8B(H8BA),
 C8C(H8CA), C8D(H8D), C9A(H9A), C9B(H9B), C9C(H9C), C9D(H9D)
5.f X=CH2 refined with riding coordinates:
 N4A(H4AA,H4AB)
5.g Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C1S(H1SM,
 H1SN,H1SO), C2S2(H2SJ,H2SK,H2SL)
5.h Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              63538
_shelx_fab_checksum              15930
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'