Unusual and Tunable Negative Linear Compressibility in the Metal-Organic Framework MFM-133(M) (M = Zr, Hf).
Yan, Yong; O'Connor, Alice E; Kanthasamy, Gopikkaa; Atkinson, George; Allan, David R.; Blake, Alexander J.; Schröder, Martin; Journal of the American Chemical Society 140 (2018) 3952–3958; doi:10.1021/jacs.7b11747

data_4131853
_publ_section_title
;
 Unusual and Tunable Negative Linear Compressibility in the Metal-Organic
 Framework MFM-133(M) (M = Zr, Hf).
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3952
_journal_page_last               3958
_journal_paper_doi               10.1021/jacs.7b11747
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.25(C184 H136 O64 Zr12)'
_chemical_formula_sum            'C46 H34 O16 Zr3'
_chemical_formula_weight         1116.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9366(11)
_cell_length_b                   18.9366(11)
_cell_length_c                   32.864(3)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.9910
_cell_measurement_theta_min      1.9450
_cell_volume                     11784.9(14)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1592
_diffrn_detector_type            'Agilent Diffraction Eos detector'
_diffrn_measured_fraction_theta_full 0.784
_diffrn_measured_fraction_theta_max 0.726
_diffrn_measurement_details
;
  1 omega    4.00   70.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870    0.0000  150.0000 66

  2 omega   -5.00   57.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  -53.0000   17.0000 62

  3 omega  -49.00  -16.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  134.0000  123.0000 33

  4 omega  -30.00   27.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   39.0000  -12.0000 57

  5 omega  -25.00   33.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   13.0000   -3.0000 58

  6 omega    8.00   74.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4874  -97.0000 -143.0000 66

  7 omega  -28.00    4.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   97.0000  -35.0000 32

  8 omega  -57.00    5.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500   53.0000  -17.0000 62

  9 omega  -14.00   15.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -81.0000   29.0000 29

 10 omega   -6.00   26.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -97.0000   35.0000 32

 11 omega  -22.00   13.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -53.0000   17.0000 35

 12 omega   -6.00   27.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -97.0000 -143.0000 33

 13 omega  -20.00   11.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   81.0000  151.0000 31

 14 omega   -7.00   70.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870  -37.0000 -180.0000 77

 15 omega  -29.00    3.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870   97.0000  -35.0000 32

 16 omega   16.00   70.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4870 -114.0000   44.0000 54

 17 omega  -52.00   17.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500   39.0000  167.0000 69

 18 omega  -25.00   29.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -39.0000   12.0000 54

 19 omega  -28.00   28.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500  -39.0000 -167.0000 56

 20 omega    3.00   37.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0500 -114.0000   44.0000 34
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, single source (Mo), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0323381278
_diffrn_orient_matrix_UB_12      -0.0011586660
_diffrn_orient_matrix_UB_13      0.0108717901
_diffrn_orient_matrix_UB_21      0.0096001891
_diffrn_orient_matrix_UB_22      0.0332400070
_diffrn_orient_matrix_UB_23      -0.0082797913
_diffrn_orient_matrix_UB_31      -0.0163170922
_diffrn_orient_matrix_UB_32      0.0172605058
_diffrn_orient_matrix_UB_33      0.0166748935
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  1.1097
_diffrn_reflns_av_unetI/netI     0.6612
_diffrn_reflns_Laue_measured_fraction_full 0.784
_diffrn_reflns_Laue_measured_fraction_max 0.726
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            92487
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.884
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.4076
_exptl_absorpt_correction_T_min  0.1242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.2378 before and 0.1083 after correction. 
The Ratio of minimum to maximum transmission is 0.3047. 
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.629
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         5206
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.3834
_refine_ls_R_factor_gt           0.1450
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3638
_refine_ls_wR_factor_ref         0.4959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1102
_reflns_number_total             5206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZrMOF_All.cif
_cod_data_source_block           28.5kbar
_cod_original_cell_volume        11784.9(18)
_cod_database_code               4131853
_chemical_oxdiff_formula         'C46 H34 O16 Zr3'
_reflns_odcompleteness_completeness 74.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C11 = C12-C11 = C8-C9
 1.39 with sigma of 0.01
 C10-C9 = C13-C11 = C2-C1
 1.5 with sigma of 0.01
 C8-C5
 1.5 with sigma of 0.01
 C12-C12_$1
 1.5 with sigma of 0.01
3. Restrained planarity
 C1_$1, C2_$1, C3_$1, C4_$1, C5_$1, C6_$1, C7_$1, C8_$1, C11_$2, C13_$2
 with sigma of 0.01
 C1_$2, C2_$2, C7_$2, C6_$2, C5_$2, C4_$2, C3_$2, C8_$2, C11_$1, C13_$1
 with sigma of 0.01
 C1_$3, C2_$3, C7_$3, C6_$3, C5_$3, C4_$3, C3_$3, C8_$3, C11, C13
 with sigma of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8, C11_$3, C13_$3
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. 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
6. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5)
7.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C10(H10A,H10B,H10C)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3)
7.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C3,C2)
;
_shelx_res_checksum              53674
_shelx_hkl_checksum              23746
_shelx_fab_checksum              61019
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'