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_7231280
_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
'C46 H33 O16 Si3 Zn3, C2 H8 N, 3.75(C3 H7 N O)'
_chemical_formula_sum            'C59.25 H67.25 N4.75 O19.75 Si3 Zn3'
_chemical_formula_weight         1442.30
_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.684(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.1888(9)
_cell_length_b                   13.9804(3)
_cell_length_c                   30.8839(8)
_cell_measurement_reflns_used    18718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0160
_cell_measurement_theta_min      2.7970
_cell_volume                     13829.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
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_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            63730
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.759
_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       needle
_exptl_crystal_F_000             5968
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         12625
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+12.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10298
_reflns_number_total             12625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00662h2.cif
_cod_data_source_block           IMP-21
_cod_depositor_comments
'Adding full bibliography for 7231278--7231280.cif.'
_cod_database_code               7231280
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              78628
_shelx_fab_checksum              7233