Siloxane-based linkers in the construction of hydrogen bonded assemblies and porous 3D MOFs
Delmas, Luke C.; Horton, Peter N.; White, Andrew J. P.; Coles, Simon J.; Lickiss, Paul D.; Davies, Robert P.; Chemical Communications  (2017) –; doi:10.1039/C7CC06022J

data_7120852
_publ_section_title
;
 Siloxane-based linkers in the construction of hydrogen bonded assemblies
 and porous 3D MOFs
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC06022J
_journal_year                    2017
_chemical_formula_moiety         'C42 H24 O16 Si2 Zn3, 7(C3 H7 N O)'
_chemical_formula_sum            'C63 H73 N7 O23 Si2 Zn3'
_chemical_formula_weight         1548.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.04 svn.r3439 for OlexSys, GUI svn.r5361)
;
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2462(5)
_cell_length_b                   27.7134(10)
_cell_length_c                   24.5341(9)
_cell_measurement_reflns_used    21610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4670
_cell_measurement_theta_min      2.2010
_cell_volume                     9006.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -78.00  73.00   1.00  120.00    --  -17.00  18.00-120.00  151
  2  \w    -87.00  22.00   1.00  120.00    --  -17.00 -72.00 -90.00  109
  3  \w    -87.00 -17.00   1.00  120.00    --  -17.00 -72.00  60.00   70
  4  \w    -75.00  -7.00   1.00  120.00    --  -17.00 -72.00-180.00   68
  5  \w    -66.00 -34.00   1.00  120.00    --  -17.00 -72.00   0.00   32
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534660000
_diffrn_orient_matrix_UB_12      -0.0001032000
_diffrn_orient_matrix_UB_13      -0.0012353000
_diffrn_orient_matrix_UB_21      0.0005404000
_diffrn_orient_matrix_UB_22      -0.0248237000
_diffrn_orient_matrix_UB_23      -0.0069787000
_diffrn_orient_matrix_UB_31      -0.0022253000
_diffrn_orient_matrix_UB_32      -0.0062067000
_diffrn_orient_matrix_UB_33      0.0280530000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.537
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       needle
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         16230
_refine_ls_number_restraints     2450
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1788P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2269
_refine_ls_wR_factor_ref         0.2552
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10870
_reflns_number_total             16230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06022j2.cif
_cod_data_source_block           IMP18
_cod_database_code               7120852
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C42 H24 Si2O13Zn3 (C3H7NO)4'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C38-C42 \\sim C40-C42 \\sim C31-C35 \\sim C33-C35 \\sim C3-C7 \\sim C5-C7
 with sigma of 0.02
 C3-C7 \\sim C5-C7 \\sim C24-C28 \\sim C26-C28 \\sim C17-C21 \\sim C19-C21
\\sim C10-C14 \\sim C12-C14
 with sigma of 0.02
 C138-C142 \\sim C140-C142 \\sim C131-C135 \\sim C133-C135 \\sim C103-C107
\\sim C105-C107
 with sigma of 0.02
 C124-C128 \\sim C126-C128 \\sim C117-C121 \\sim C119-C121 \\sim C110-C114
\\sim C112-C114
 with sigma of 0.02
4. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, Si1
 with sigma of 0.01
 C8, C9, C10, C11, C12, C13, C14, Si1
 with sigma of 0.01
 C15, C16, C17, C18, C19, C20, C21, Si1
 with sigma of 0.01
 C22, C23, C24, C25, C26, C27, C28, Si2
 with sigma of 0.01
 C29, C30, C31, C32, C33, C34, C35, Si2
 with sigma of 0.01
 C36, C37, C38, C39, C40, C41, C42, Si2
 with sigma of 0.01
 C101, C102, C103, C104, C105, C106, C107, Si11
 with sigma of 0.01
 C108, C109, C110, C111, C112, C113, C114, Si11
 with sigma of 0.01
 C115, C116, C117, C118, C119, C120, C121, Si11
 with sigma of 0.01
 C122, C123, C124, C125, C126, C127, C128, Si12
 with sigma of 0.01
 C129, C130, C131, C132, C133, C134, C135, Si12
 with sigma of 0.01
 C136, C137, C138, C139, C140, C141, C142, Si12
 with sigma of 0.01
5. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(O9) = Uanis(O13)
Uanis(O104) = Uanis(O105)
7. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Same fragment restrains
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
C34, C35, C36, C37, C38, C39, C40, C41, C42, O1, O2, O3, O4, O5, O6, O7, O8,
O9, O10, O11, O12, O13, Si1, Si2} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, C102, C103, C104, C105, C106, C107, C108, C109, C110, C111, C112, C113,
C114, C115, C116, C117, C118, C119, C120, C121, C122, C123, C124, C125, C126,
C127, C128, C129, C130, C131, C132, C133, C134, C135, C136, C137, C138, C139,
C140, C141, C142, O101, O102, O103, O104, O105, O106, O107, O108, O109, O110,
O111, O112, O113, Si11, Si12}
9. Others
 Fixed Sof: Zn11(0.5) Zn12(0.5) O51(0.5) O52(0.5) C1(0.5) C2(0.5) H2(0.5)
 C3(0.5) H3(0.5) C4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5)
 C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5)
 C14(0.5) C15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) C19(0.5)
 H19(0.5) C20(0.5) H20(0.5) C21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) C29(0.5)
 C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) C33(0.5) H33(0.5) C34(0.5)
 H34(0.5) C35(0.5) C36(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5)
 C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5)
 O5(0.5) O6(0.5) O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5) O12(0.5) O13(0.5)
 Si1(0.5) Si2(0.5) C101(0.5) C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5)
 C105(0.5) H105(0.5) C106(0.5) H106(0.5) C107(0.5) C108(0.5) C109(0.5)
 H109(0.5) C110(0.5) H110(0.5) C111(0.5) C112(0.5) H112(0.5) C113(0.5)
 H113(0.5) C114(0.5) C115(0.5) C116(0.5) H116(0.5) C117(0.5) H117(0.5)
 C118(0.5) C119(0.5) H119(0.5) C120(0.5) H120(0.5) C121(0.5) C122(0.5)
 C123(0.5) H123(0.5) C124(0.5) H124(0.5) C125(0.5) C126(0.5) H126(0.5)
 C127(0.5) H127(0.5) C128(0.5) C129(0.5) C130(0.5) H130(0.5) C131(0.5)
 H131(0.5) C132(0.5) C133(0.5) H133(0.5) C134(0.5) H134(0.5) C135(0.5)
 C136(0.5) C137(0.5) H137(0.5) C138(0.5) H138(0.5) C139(0.5) C140(0.5)
 H140(0.5) C141(0.5) H141(0.5) C142(0.5) O101(0.5) O102(0.5) O103(0.5)
 O104(0.5) O105(0.5) O106(0.5) O107(0.5) O108(0.5) O109(0.5) O110(0.5)
 O111(0.5) O112(0.5) O113(0.5) Si11(0.5) Si12(0.5)
10.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27),
  C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40),
 C41(H41), C102(H102), C103(H103), C105(H105), C106(H106), C109(H109),
 C110(H110), C112(H112), C113(H113), C116(H116), C117(H117), C119(H119),
 C120(H120), C123(H123), C124(H124), C126(H126), C127(H127), C130(H130),
 C131(H131), C133(H133), C134(H134), C137(H137), C138(H138), C140(H140),
 C141(H141)
10.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C8(C9,C10,C11,C12,C13), C15(C16,C17,C18,C19,C20), C22(C23,
 C24,C25,C26,C27), C29(C30,C31,C32,C33,C34), C36(C37,C38,C39,C40,C41),
 C101(C102,C103,C104,C105,C106), C108(C109,C110,C111,C112,C113), C115(C116,C117,
 C118,C119,C120), C122(C123,C124,C125,C126,C127), C129(C130,C131,C132,C133,
 C134), C136(C137,C138,C139,C140,C141)
;
_shelx_res_checksum              94135
_shelx_fab_checksum              20642
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.760