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_7120850
_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 H30 O13 Si2, 2(C2 H4 O2)'
_chemical_formula_sum            'C46 H38 O17 Si2'
_chemical_formula_weight         918.94
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                93.458(3)
_cell_angle_beta                 105.795(4)
_cell_angle_gamma                104.490(3)
_cell_formula_units_Z            4
_cell_length_a                   17.0954(9)
_cell_length_b                   17.1816(4)
_cell_length_c                   17.3736(7)
_cell_measurement_reflns_used    5553
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.3800
_cell_measurement_theta_min      4.0100
_cell_volume                     4708.8(4)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28020
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.883
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       tablets
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1056
_refine_ls_number_reflns         18029
_refine_ls_number_restraints     496
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1224P)^2^+0.6651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2206
_refine_ls_wR_factor_ref         0.2750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10623
_reflns_number_total             18029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06022j2.cif
_cod_data_source_block           L1-H6
_cod_database_code               7120850
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              21860
_shelx_fab_checksum              69837