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_7043863
_publ_section_title
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 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
(HNEt3)[Mn(III)5(mu3-O)2(CH3COO)4(L1)4].4CH3CN.4H2O
_chemical_formula_sum            'C62 H84 Mn5 N25 O22'
_chemical_formula_weight         1806.24
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-21
_audit_creation_method
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Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.658(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1753(12)
_cell_length_b                   23.756(3)
_cell_length_c                   26.951(3)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.40
_cell_volume                     7757.2(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            117295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         1.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0486 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.9055.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear brownish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         13738
_refine_ls_number_restraints     1097
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0400P)^2^+17.4740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11600
_reflns_number_total             13738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02430d2.cif
_cod_data_source_block           Mn5L1
_cod_original_cell_volume        7757.0(14)
_cod_database_code               7043863
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4A-H4AA = N4A-H4AB = N4C-H4CA = N4C-H4CB = N4B-H4BB = N4B-H4BA = N4D-H4DB =
 N4D-H4DA
 0.86 with sigma of 0.02
 O1S-H1SH = O1S-H1SG
 0.85 with sigma of 0.02
 N5SA-C5SC = N5SB-C5SD
 2.67 with sigma of 0.02
 C5SD-C5SB \\sim C5SA_$1-C5SC_$1
 with sigma of 0.02
 N5SB-C5SB \\sim N5SA_$1-C5SA_$1
 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
 Sof(N5SA)=Sof(C5SA)=Sof(C5SC)=1-FVAR(1)
 Sof(N5SB)=Sof(C5SB)=Sof(C5SD)=FVAR(1)
 Sof(O5S)=1-FVAR(2)
 Sof(O4S)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 N1S(H1S)
5.b Secondary CH2 refined with riding coordinates:
 C1SA(H1SA,H1SB), C1SB(H1SC,H1SD), C1SC(H1SE,H1SF)
5.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C7A(H7A), C8A(H8AA), C9A(H9A), C3B(H3B), C7B(H7B), C8B(H8BA),
 C9B(H9B), C3C(H3C), C7C(H7C), C8C(H8CA), C9C(H9C), C3D(H3D), C7D(H7D),
 C8D(H8D), C9D(H9D)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10A(H10A,
 H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G,H10H,H10I), C10D(H10J,H10K,H10L),
 C2SA(H2SA,H2SB,H2SC), C2SB(H2SD,H2SE,H2SF), C2SC(H2SG,H2SH,H2SI), C4S2(H4SA,
 H4SB,H4SC), C3S2(H3SA,H3SB,H3SC), C2S2(H2SJ,H2SK,H2SL)
;
_shelx_res_checksum              73141
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'