Metal-Organic Frameworks Based on Tri- and Penta-nuclear Manganese(II) Secondary Building Units Self-assembled by a V-Shaped Silicon-containing Dicarboxylate
Vlad, Angelica; Zaltariov, Mirela-Fernanda; Sova, Sergiu; Novitchi, Ghénadie; Train, Cyrille; Cazacu, Maria; RSC Adv.  (2016) –; doi:10.1039/C6RA03969C

data_7224877
_publ_section_title
;
 Metal-Organic Frameworks Based on Tri- and Penta-nuclear Manganese(II)
 Secondary Building Units Self-assembled by a V-Shaped Silicon-containing
 Dicarboxylate
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA03969C
_journal_year                    2016
_chemical_formula_moiety         'C118 H106 Mn5 N4 O26 Si4, 6(C3 H7 N O)'
_chemical_formula_sum            'C136 H148 Mn5 N10 O32 Si4'
_chemical_formula_weight         2821.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4767)
;
_audit_update_record
;
2016-02-04 deposited with the CCDC.
2016-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                64.428(4)
_cell_angle_beta                 82.624(3)
_cell_angle_gamma                68.486(4)
_cell_formula_units_Z            1
_cell_length_a                   15.2389(6)
_cell_length_b                   15.9970(7)
_cell_length_c                   17.4713(7)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      29.3813
_cell_measurement_theta_min      2.3847
_cell_volume                     3571.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.05(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -80.00   -1.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -57.0000 -120.0000 79

  2 omega  -76.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -57.0000   90.0000 73

  3 omega  -24.00   19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000   30.0000 43

  4 omega   12.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789   57.0000 -120.0000 28

  5 omega  -29.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789   57.0000    0.0000 81

  6 omega  -74.00  -19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -57.0000 -180.0000 55

  7 omega   35.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5133  178.0000 -180.0000 45

  8 omega  -31.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789   38.0000 -150.0000 86

  9 omega   32.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5133 -178.0000   30.0000 55
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0101197000
_diffrn_orient_matrix_UB_12      0.0450245000
_diffrn_orient_matrix_UB_13      -0.0370397000
_diffrn_orient_matrix_UB_21      -0.0189859000
_diffrn_orient_matrix_UB_22      -0.0196117000
_diffrn_orient_matrix_UB_23      -0.0206350000
_diffrn_orient_matrix_UB_31      -0.0452043000
_diffrn_orient_matrix_UB_32      0.0183653000
_diffrn_orient_matrix_UB_33      0.0151803000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40308
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         5.11
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1471
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         13395
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+4.0394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2331
_reflns_number_gt                8537
_reflns_number_total             13395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra03969c2.cif
_cod_data_source_block           shi_1662_av
_cod_database_code               7224877
_chemical_oxdiff_formula         'C30 H30 O8 Mn2 Si1'
_chemical_oxdiff_usercomment     'AV_131, incolore, 0.4x0.4x0.3'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N2-C1Z = N2-C1Y = N2X-C62 = N2X-C61
 1.47 with sigma of 0.01
 C1Z-C60X = C60X-C1Y
 2.42 with sigma of 0.001
 O11-O11X
 0.5 with sigma of 0.01
 N3-C71X = N3-C70X
 1.47 with sigma of 0.01
 N3-C69X
 1.36 with sigma of 0.01
 C71X-C69X = C69X-C70X
 2.4 with sigma of 0.01
 N3X-C69
 1.36 with sigma of 0.01
 N3X-C71 = N3X-C70
 1.47 with sigma of 0.01
 C71-C69 = C69-C70
 2.4 with sigma of 0.01
 O14X-C69X = O14-C69
 1.2 with sigma of 0.01
 N2-C60X = N2X-C60
 1.38 with sigma of 0.01
 C61-C60 = C60-C62
 2.42 with sigma of 0.001
 O11X-C60X = O11-C60
 1.2 with sigma of 0.01
 N4-C65X \\sim N4-C64 \\sim N1-C56 \\sim N1-C55 \\sim N5-C59 \\sim N5-C58
 with sigma of 0.01
 Mn2-O11X \\sim Mn2-O11
 with sigma of 0.001
 N4-C65X \\sim N4-C65
 with sigma of 0.001
3. Restrained planarity
 C60X, N2, C1Z, C1Y
 with sigma of 0.1
 O14X, C69X, N3, C70X, C71X
 with sigma of 0.01
 O14, C69, N3X, C70, C71
 with sigma of 0.01
 C60, N2X, C61, C62
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C65X) = Uiso(C65)
Uiso(C71X) = Uiso(C71) = Uiso(N3) = Uiso(C70X) = Uiso(O14X) = Uiso(C70) =
Uiso(C69X) = Uiso(C69) = Uiso(O14) = Uiso(N3X)
Uiso(O11X) = Uiso(O11) = Uiso(C60) = Uiso(C60X) = Uiso(N2) = Uiso(C1Y) =
Uiso(C1Z) = Uiso(N2X) = Uiso(C62) = Uiso(C61)
5. Others
 Fixed Sof: N3X(0.5) C69(0.5) H69(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5)
 O14(0.5) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5) C65X(0.5) H65A(0.5) H65B(0.5)
 H65C(0.5) O11(0.5) O11X(0.5) N2X(0.5) C60(0.5) H60(0.5) N3(0.5) C71X(0.5)
 H71D(0.5) H71E(0.5) H71F(0.5) C70X(0.5) H70D(0.5) H70E(0.5) H70F(0.5)
 O14X(0.5) C69X(0.5) H69X(0.5) N2(0.5) C1Y(0.5) H1YA(0.5) H1YB(0.5) H1YC(0.5)
 C1Z(0.5) H1ZA(0.5) H1ZB(0.5) H1ZC(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C60X(0.5) H60X(0.5) C65(0.5) H65D(0.5)
 H65E(0.5) H65F(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), C55(H55A,H55B,H55C), C64(H64A,H64B,H64C), C56(H56A,H56B,H56C),
  C71(H71A,H71B,H71C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C70(H70A,H70B,
 H70C), C65X(H65A,H65B,H65C), C71X(H71D,H71E,H71F), C70X(H70D,H70E,H70F),
 C65(H65D,H65E,H65F)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C7(H7), C30(H30), C29(H29), C33(H33), C10(H10), C32(H32), C4(H4),
 C6(H6), C51(H51), C50(H50), C47(H47), C13(H13), C3(H3), C39(H39), C16(H16),
 C48(H48), C42(H42), C17(H17), C22(H22), C26(H26), C20(H20), C41(H41), C19(H19),
  C18(H18), C23(H23), C44(H44), C35(H35), C45(H45), C53(H53), C57(H57),
 C43(H43), C69(H69), C54(H54), C9(H9), C25(H25), C24(H24), C37(H37), C36(H36),
 C38(H38), C63(H63), C60(H60), C69X(H69X), C60X(H60X)
6.c Idealised Me refined as rotating group:
 C1Y(H1YA,H1YB,H1YC), C1Z(H1ZA,H1ZB,H1ZC), C62(H62A,H62B,H62C), C61(H61A,H61B,
 H61C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'