Liquid exfoliation of alkyl-ether functionalised layered metal-organic frameworks to nanosheets.
Foster, Jonathan A.; Henke, Sebastian; Schneemann, Andreas; Fischer, Roland A.; Cheetham, Anthony K.; Chemical communications (Cambridge, England) 52 (2016) 10474–10477; doi:10.1039/c6cc05154e

data_7124852
_publ_section_title
;
 Liquid exfoliation of alkyl-ether functionalised layered metal-organic
 frameworks to nanosheets.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10474
_journal_page_last               10477
_journal_paper_doi               10.1039/c6cc05154e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C19 H27 N O9 Zn'
_chemical_formula_sum            'C19 H27 N O9 Zn'
_chemical_formula_weight         478.78
_chemical_name_systematic        Zn(BMP-bdc)(DMF)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-08
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-08 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                85.208(3)
_cell_angle_beta                 74.992(3)
_cell_angle_gamma                67.508(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4273(6)
_cell_length_b                   10.8211(5)
_cell_length_c                   10.8805(3)
_cell_measurement_reflns_used    4861
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      28.7906
_cell_measurement_theta_min      3.2489
_cell_volume                     1095.45(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
  1 omega  -73.00  111.00   1.0000   25.0800
omega____ theta____ kappa____ phi______ frames
    -       20.6944    6.0000   97.0000 184

  2 omega   62.00  120.00   1.0000   25.0800
omega____ theta____ kappa____ phi______ frames
    -       20.6944  179.0000  120.0000 58

  3 omega   59.00   95.00   1.0000   25.0800
omega____ theta____ kappa____ phi______ frames
    -       20.6944  179.0000 -150.0000 36

  4 omega -100.00  -56.00   1.0000   25.0800
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  179.0000 -180.0000 44

  5 omega -121.00  -54.00   1.0000   25.0800
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  179.0000   90.0000 67
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0617112092
_diffrn_orient_matrix_UB_12      -0.0151606386
_diffrn_orient_matrix_UB_13      0.0057639801
_diffrn_orient_matrix_UB_21      0.0423792643
_diffrn_orient_matrix_UB_22      -0.0693019569
_diffrn_orient_matrix_UB_23      -0.0009521555
_diffrn_orient_matrix_UB_31      -0.0128323164
_diffrn_orient_matrix_UB_32      0.0015086088
_diffrn_orient_matrix_UB_33      0.0672358759
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7710
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.854
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
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    1.452
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_recrystallization_method 'Solvothermal Synthesis'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0284P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3981
_reflns_number_total             4844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05154e2.cif
_cod_data_source_block           zn-bmp-bdc-dmf
_cod_original_cell_volume        1095.45(9)
_cod_database_code               7124852
_chemical_oxdiff_formula         'C12 H10 S O2'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C17(H17)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'