Unusual Mn(III/IV)4 Cubane and Mn(III)16M4 (M = Ca, Sr) Looplike Clusters from the Use of Dimethylarsinic Acid.
Chakov, Nicole E.; Thuijs, Annaliese E.; Wernsdorfer, Wolfgang; Rheingold, Arnold L.; Abboud, Khalil A.; Christou, George; Inorganic chemistry 55 (2016) 8468–8477; doi:10.1021/acs.inorgchem.6b01077

data_4348219
_publ_section_title
;
 Unusual Mn(III/IV)4 Cubane and Mn(III)16M4 (M = Ca, Sr) Looplike Clusters
 from the Use of Dimethylarsinic Acid.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8468
_journal_page_last               8477
_journal_paper_doi               10.1021/acs.inorgchem.6b01077
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C12 H36 As6 Mn4 O16, 7(H2 O)'
_chemical_formula_sum            'C12 H50 As6 Mn4 O23'
_chemical_formula_weight         1231.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                99.8690(10)
_cell_angle_beta                 90.4520(10)
_cell_angle_gamma                111.7540(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7278(7)
_cell_length_b                   13.7179(8)
_cell_length_c                   14.0559(9)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.29
_cell_volume                     2062.9(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      218.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15304
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.475
_exptl_absorpt_coefficient_mu    6.042
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.231
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9507
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+7.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8006
_reflns_number_total             9507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01077_si_001.cif
_cod_data_source_block           chr12x
_cod_database_code               4348219
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O17-H17B = O17-H17A
 0.9 with sigma of 0.001
 O18-H18A = O18-H18B
 0.9 with sigma of 0.001
 O19-H19B = O19-H19A
 0.9 with sigma of 0.001
 O1AA-H1AA = O1AA-H1AB
 0.9 with sigma of 0.001
 O21-H21 = O21-H21A
 0.9 with sigma of 0.001
 O0AA-H0AB = O0AA-H0AA
 0.9 with sigma of 0.001
 O20-H20A = O20-H20
 0.9 with sigma of 0.001
 H17B-H17A
 1.45 with sigma of 0.001
 H18A-H18B
 1.45 with sigma of 0.001
 H19B-H19A
 1.45 with sigma of 0.04
 H1AA-H1AB
 1.45 with sigma of 0.001
 H21-H21A
 1.45 with sigma of 0.001
 H0AB-H0AA
 1.45 with sigma of 0.001
 H20-H20A
 1.45 with sigma of 0.001
3. Others
 Fixed Uiso: H19B(0.15) H1AA(0.15) H21A(0.1) H20A(0.15) H20(0.155)
4.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              86324
_shelx_hkl_checksum              77129
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'