Trisiloxane-centred metal‒organic frameworks and hydrogen bonded assemblies
Delmas, Luke C.; White, Andrew J. P.; Pugh, David; Horton, Peter N.; Coles, Simon J.; Lickiss, Paul D.; Davies, Robert P.; CrystEngComm 20 (2018) 4541–; doi:10.1039/C8CE00662H

data_7231278
_publ_section_title
;
 Trisiloxane-centred metal--organic frameworks and hydrogen bonded
 assemblies
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4541
_journal_paper_doi               10.1039/C8CE00662H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C44 H36 O14 Si3, C2 H4 O2, 0.5(H2O)'
_chemical_formula_sum            'C46 H41 O16.5 Si3'
_chemical_formula_weight         942.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.516(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1118(4)
_cell_length_b                   15.4367(5)
_cell_length_c                   40.6572(13)
_cell_measurement_reflns_used    6164
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.4110
_cell_measurement_theta_min      4.0810
_cell_volume                     9440.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'enCIFer, Platon'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    Olex-2
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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     17.00 100.00   1.00   14.03    --   41.86  38.00 -90.00   83
  2  \w     83.00 177.00   1.00   64.84    --  106.38  61.00-120.00   94
  3  \w     95.00 178.00   1.00   64.84    --  106.38  30.00 -30.00   83
  4  \w    125.00 176.00   1.00   64.84    --  106.38 125.00  90.00   51
  5  \w     73.00 101.00   1.00   64.84    --  106.38 125.00  90.00   28
  6  \w     33.00 133.00   1.00   64.84    --  106.38 -77.00 120.00  100
  7  \w    -73.00  19.00   1.00   14.03    --  -41.86  77.00  60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            29868
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         6.446
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97847
_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    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         16505
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1230P)^2^+14.0199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12216
_reflns_number_total             16505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00662h2.cif
_cod_data_source_block           ligand_L
_cod_depositor_comments
'Adding full bibliography for 7231278--7231280.cif.'
_cod_original_formula_sum        'C46 H41 O16.50 Si3'
_cod_database_code               7231278
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.914
_oxdiff_exptl_absorpt_empirical_full_min 0.927
_oxdiff_exptl_absorpt_empirical_full_max 1.096
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              88772