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_7224878
_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
'0.5(C220 H184 Mn6 N4 O40 Si8), 2(C3 H7 N O), 12(H2 O)'
_chemical_formula_sum            'C116 H130 Mn3 N4 O34 Si4'
_chemical_formula_weight         2401.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2016-02-04 deposited with the CCDC.
2016-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.328(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.5500(11)
_cell_length_b                   17.3564(5)
_cell_length_c                   30.9789(13)
_cell_measurement_reflns_used    8011
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      25.4360
_cell_measurement_theta_min      1.6840
_cell_volume                     12794.7(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      173.05(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -81.00  -35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127 -178.0000   90.0000 46

  2 omega   43.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908  178.0000  120.0000 26

  3 omega  -42.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908  -38.0000  -30.0000 86

  4 omega   -4.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908   77.0000  120.0000 83

  5 omega  -25.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908  -99.0000  -30.0000 32

  6 omega  -10.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5908   77.0000  -60.0000 61
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0231290000
_diffrn_orient_matrix_UB_12      0.0234156000
_diffrn_orient_matrix_UB_13      0.0147928000
_diffrn_orient_matrix_UB_21      0.0187048000
_diffrn_orient_matrix_UB_22      -0.0270158000
_diffrn_orient_matrix_UB_23      -0.0023289000
_diffrn_orient_matrix_UB_31      -0.0018703000
_diffrn_orient_matrix_UB_32      0.0198030000
_diffrn_orient_matrix_UB_33      -0.0206903000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39561
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5028
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.283
_refine_diff_density_min         -1.987
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         12496
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+27.1482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1994
_reflns_number_gt                8874
_reflns_number_total             12496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra03969c2.cif
_cod_data_source_block           shi_2197_av
_cod_original_cell_volume        12794.7(8)
_cod_database_code               7224878
_chemical_oxdiff_formula         'C20 H40 N6 O8 Si3 Mn1'
_chemical_oxdiff_usercomment     Mn3
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H11A,H11B} of O11W, {H1WA,H1WB} of O1W
 At 1.5 times of:
  All C(H,H,H) groups, {H19A,H19B} of O19W, {H14A,H14B} of O14W, {H9WA,H9WB}
  of O9W, {H7WA,H7WB} of O7W, {H2WA,H2WB} of O2W, {H3WA,H3WB} of O3W, {H5WA,
  H5WB} of O5W, {H4WA,H4WB} of O4W, {H16A,H16B} of O16W, {H17A,H17B} of O17W,
  {H18A,H18B} of O18W, {H12A,H12B} of O12W, {H10A,H10B} of O10W, {H13A,H13B} of
  O13W, {H6WA,H6WB} of O6W, All O(H) groups
2. Restrained distances
 C60-C61
 2.5 with sigma of 0.01
 O10-C56
 1.2 with sigma of 0.001
 O1W-H1WA = O1W-H1WB
 0.86 with sigma of 0.01
 N2-C58 = N2-C57
 1.46 with sigma of 0.001
 O1W-H1WA \\sim O1W-H1WB
 with sigma of 0.01
3. Restrained planarity
 O10, C56, N2, C57, C58
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(O19W) = Uiso(O7W) = Uiso(O17W) = Uiso(O18W) = Uiso(O6W) = Uiso(O16W)
Uiso(O14W) = Uiso(O11) = Uiso(C59) = Uiso(O11W) = Uiso(N3) = Uiso(C60) =
Uiso(C61) = Uiso(O12W) = Uiso(O13W)
Uiso(O10) = Uiso(C56) = Uiso(N2) = Uiso(C57) = Uiso(O10W) = Uiso(C58) =
Uiso(O9W)
5. Others
 Fixed Sof: H4(0.5) H8(0.5) O11(0.5) N3(0.5) C59(0.5) H59(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) N2(0.5)
 C56(0.5) H56(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) H58C(0.5) O10W(0.25) H10A(0.25) H10B(0.25) O13W(0.15) H13A(0.15)
 H13B(0.15) O11W(0.2) H11A(0.2) H11B(0.2) O6W(0.35) H6WA(0.35) H6WB(0.35)
 O7W(0.25) H7WA(0.25) H7WB(0.25) O9W(0.25) H9WA(0.25) H9WB(0.25) O14W(0.2)
 H14A(0.2) H14B(0.2) O5W(0.75) H5WA(0.75) H5WB(0.75) O19W(0.1) H19A(0.1)
 H19B(0.1) O18W(0.1) H18A(0.1) H18B(0.1) O12W(0.15) H12A(0.15) H12B(0.15)
 O17W(0.15) H17A(0.15) H17B(0.15) O16W(0.1) H16A(0.1) H16B(0.1)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O4(H4), O8(H8), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C56(H56), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), O10W(H10A,H10B), O13W(H13A,H13B), O11W(H11A,H11B),
 O6W(H6WA,H6WB), O7W(H7WA,H7WB), O9W(H9WA,H9WB), O14W(H14A,H14B), O5W(H5WA,
 H5WB), O4W(H4WA,H4WB), O3W(H3WA,H3WB), O2W(H2WA,H2WB), O19W(H19A,H19B),
 O18W(H18A,H18B), O12W(H12A,H12B), O17W(H17A,H17B), O16W(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35),
 C36(H36), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C59(H59)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'