Hierarchical Assembly of a {Mn(II)15Mn(III)4} Brucite Disc: Step-by-Step Formation and Ferrimagnetism.
Deng, Yong-Kai; Su, Hai-Feng; Xu, Jia-Heng; Wang, Wen-Guang; Kurmoo, Mohamedally; Lin, Shui-Chao; Tan, Yuan-Zhi; Jia, Jiong; Sun, Di; Zheng, Lan-Sun; Journal of the American Chemical Society 138 (2016) 1328–1334; doi:10.1021/jacs.5b11736

data_4124876
_publ_section_title
;
 Hierarchical Assembly of a {Mn(II)15Mn(III)4} Brucite Disc: Step-by-Step
 Formation and Ferrimagnetism.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1328
_journal_page_last               1334
_journal_paper_doi               10.1021/jacs.5b11736
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C132 H210 Cl6 Mn19 N66 O54'
_chemical_formula_weight         4842.22
_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'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   35.950(6)
_cell_length_b                   35.950
_cell_length_c                   13.522(2)
_cell_measurement_reflns_used    1130
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      43.349
_cell_measurement_theta_min      4.532
_cell_volume                     15135(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_sigmaI/netI    0.1928
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22912
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_correction_T_min  0.8276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7419
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6935
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.2127
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                2704
_reflns_number_total             6935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b11736_si_002.cif
_cod_data_source_block           p
_cod_depositor_comments
;
          Adding full bibliography for 4124876.cif.

2021-04-11
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_cell_volume        15134(4)
_cod_database_code               4124876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O6 \\sim Cl1 \\sim O7 \\sim O8 \\sim O9: within 1.7A with sigma of 0.002 and
sigma for terminal atoms of 0.08
3.a Ternary CH refined with riding coordinates:
 O4(H4), O5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
3.c Me refined with riding coordinates:
 C20(H20A,H20B,H20C)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C15(H15)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'