Synthesis of new Mn<sub>19</sub> analogues and their structural, electrochemical and catalytic properties.
Chevallot-Beroux, Elodie; Ako, Ayuk M.; Schmitt, Wolfgang; Twamley, Brendan; Moran, Joseph; Corinne, Boudon; Ruhlmann, Laurent; Mameri, Samir; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4830–4836; doi:10.1039/c8dt04807j

data_7701718
_publ_section_title
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 Synthesis of new Mn<sub>19</sub> analogues and their structural,
 electrochemical and catalytic properties.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4830
_journal_page_last               4836
_journal_paper_doi               10.1039/c8dt04807j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C120 H126 Cl8 Mn18 N6 O44 Sr1, 7(C H4 O)'
_chemical_formula_sum            'C127 H154 Cl8 Mn18 N6 O51 Sr'
_chemical_formula_weight         3940.69
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-11-30 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.6642(8)
_cell_length_b                   20.6642(8)
_cell_length_c                   35.2511(15)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.55
_cell_volume                     13035.9(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2013)'
_computing_data_collection       'APEX 3 (Bruker, 2016) '
_computing_data_reduction        'SAINT v8.37A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker D8 Quest ECO'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            62285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'standard sealed x-ray tube'
_diffrn_source_target            Mok\a
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0758 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8947. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             5970
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.892
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+142.7258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4558
_reflns_number_total             5943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04807j2.cif
_cod_data_source_block           tcd716
_cod_original_cell_volume        13035.9(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7701718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.731
_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) groups
2. Restrained distances
 O00W-C4 = O00Y-C3 = O012-C2
 1.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O00W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(O012) \\sim Ueq, Uanis(O00Y) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(O00W) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O00W(0.5) H00W(0.5) O00Y(0.16667) H00Y(0.16667) O012(0.5)
 H012(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.16667) H3B(0.16667)
 H3C(0.16667) H3A(0.16667) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
5.a Riding coordinates:
 O00Y(H00Y), C2(H2A,H2B,H2C), C3(H3B,H3C,H3A), C4(H4A,H4B,H4C)
5.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00K(H00C,H00D), C00M(H00E,H00F), C00Q(H00G,H00H)
5.c Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00T(H00T), C00U(H00U)
5.d Idealised Me refined as rotating group:
 C00X(H00I,H00J,H00K), C00Z(H00L,H00M,H00O), C011(H01A,H01B,H01C)
5.e Idealised tetrahedral OH refined as rotating group:
 O00W(H00W), O012(H012)
;
_shelx_res_checksum              93633
_olex2_exptl_crystal_mounting_method 'mounted in oil on a Mitegen holder'
_olex2_submission_original_sample_id TCD373c
_olex2_submission_special_instructions 'No special instructions were received'