Synthesis and crystal structure of a Mn-based coordination complex as precursor for the synthesis of Mn2O3
Wang, Ao; Huang, Peng-Bin; Sun, Ping-Ping; Shi, Fa-Nian; Tian, Bo; Gao, Jun; Inorganica Chimica Acta 498 (2019) 119166–; doi:10.1016/j.ica.2019.119166

data_1565789
_publ_section_title
;
 Synthesis and crystal structure of a Mn-based coordination complex as
 precursor for the synthesis of Mn2O3
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119166
_journal_paper_doi               10.1016/j.ica.2019.119166
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C68 H66 Mn2 N8 O9, 3.5(H2 O), H O'
_chemical_formula_sum            'C68 H75 Mn2 N8 O13.5'
_chemical_formula_weight         1330.24
_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
_cell_angle_alpha                89.7240(10)
_cell_angle_beta                 88.5610(10)
_cell_angle_gamma                85.7360(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9986(2)
_cell_length_b                   12.8222(2)
_cell_length_c                   20.1046(3)
_cell_measurement_reflns_used    26725
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.2090
_cell_measurement_theta_min      3.5760
_cell_volume                     3083.51(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64407
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.630
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.9715
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.747
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         11187
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0720P)^2^+5.6913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9314
_reflns_number_total             11187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119166.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C68 H75 Mn2 N8 O13.50'
_cod_database_code               1565789
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.972
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O10-H10B = O11-H11A = O11-H11B
 0.82 with sigma of 0.02
 O11-H11A = O11-H11B
 0.78 with sigma of 0.02
 O12-H12A = O12-H12B
 0.7 with sigma of 0.02
 H12A-H12B
 1.2 with sigma of 0.02
3. Others
 Fixed Sof: O13(0.5)
4.a Riding coordinates:
 O13(H13), O14(H14A)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
  C66(H66A,H66B), C67(H67A,H67B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C0AA(H0AA),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C35(H35),
  C36(H36), C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
 C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56)
;