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_4131861
_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                   18.779(3)
_cell_length_b                   18.779(3)
_cell_length_c                   33.087(7)
_cell_measurement_reflns_used    4312
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.3680
_cell_measurement_theta_min      1.9520
_cell_volume                     11668(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1592
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.676
_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      4.00  70.00   1.00  120.00    --   26.49   0.00 150.00   66
  2  \w     -5.00  57.00   1.00  120.00    --   26.49 -53.00  17.00   62
  3  \w    -49.00 -16.00   1.00  120.00    --   26.49 134.00 123.00   33
  4  \w    -30.00  27.00   1.00  120.00    --   26.49  39.00 -12.00   57
  5  \w    -25.00  33.00   1.00  120.00    --   26.49  13.00  -3.00   58
  6  \w      8.00  74.00   1.00  120.00    --   26.49 -97.00-143.00   66
  7  \w    -28.00   4.00   1.00  120.00    --   26.49  97.00 -35.00   32
  8  \w    -57.00   5.00   1.00  120.00    --  -28.05  53.00 -17.00   62
  9  \w    -14.00  15.00   1.00  120.00    --  -28.05 -81.00  29.00   29
 10  \w     -6.00  26.00   1.00  120.00    --  -28.05 -97.00  35.00   32
 11  \w    -22.00  13.00   1.00  120.00    --  -28.05 -53.00  17.00   35
 12  \w     -6.00  27.00   1.00  120.00    --  -28.05 -97.00-143.00   33
 13  \w    -20.00  11.00   1.00  120.00    --   26.49  81.00 151.00   31
 14  \w     -7.00  70.00   1.00  120.00    --   26.49 -37.00-180.00   77
 15  \w    -29.00   3.00   1.00  120.00    --   26.49  97.00 -35.00   32
 16  \w     16.00  70.00   1.00  120.00    --   26.49-114.00  44.00   54
 17  \w    -52.00  17.00   1.00  120.00    --  -28.05  39.00 167.00   69
 18  \w    -25.00  29.00   1.00  120.00    --  -28.05 -39.00  12.00   54
 19  \w    -28.00  28.00   1.00  120.00    --  -28.05 -39.00-167.00   56
 20  \w      3.00  37.00   1.00  120.00    --  -28.05-114.00  44.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0329324000
_diffrn_orient_matrix_UB_12      0.0010897000
_diffrn_orient_matrix_UB_13      0.0104865000
_diffrn_orient_matrix_UB_21      -0.0095601000
_diffrn_orient_matrix_UB_22      -0.0332713000
_diffrn_orient_matrix_UB_23      -0.0085900000
_diffrn_orient_matrix_UB_31      0.0158455000
_diffrn_orient_matrix_UB_32      -0.0178433000
_diffrn_orient_matrix_UB_33      0.0166341000
_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  0.6072
_diffrn_reflns_av_unetI/netI     0.4285
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.676
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            83282
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.809
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.4062
_exptl_absorpt_correction_T_min  0.2757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.2070 before and 0.0947 after correction. 
The Ratio of minimum to maximum transmission is 0.6787. 
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    0.636
_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         1.177
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         4763
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.3020
_refine_ls_R_factor_gt           0.1109
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_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          0.2928
_refine_ls_wR_factor_ref         0.3934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1170
_reflns_number_total             4763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZrMOF_All.cif
_cod_data_source_block           44.7kbar
_cod_database_code               4131861
_chemical_oxdiff_formula         'C44 H36 O8 Zr'
_chemical_oxdiff_usercomment     'GA009 @ 40.9 kbar'
_reflns_odcompleteness_completeness 70.35
_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
 C9-C10 = C13-C11
 1.5 with sigma of 0.01
 C12-C11 = C8-C11 = C9-C8
 1.39 with sigma of 0.01
 C8-C5
 1.5 with sigma of 0.01
 C13_$1-C11_$1
 1.5 with sigma of 0.01
 C12-C12_$3
 1.5 with sigma of 0.01
 C2-C1
 1.5 with sigma of 0.01
3. Restrained planarity
 C1, C2, C7, C6, C5, C4, C3, C8, C11_$1, C13_$1
 with sigma of 0.005
 C1_$1, C2_$1, C3_$1, C7_$1, C6_$1, C5_$1, C4_$1, C8_$1, C11, C13
 with sigma of 0.005
 C1_$2, C2_$2, C3_$2, C4_$2, C5_$2, C6_$2, C7_$2, C8_$2, C11_$3, C13_$3
 with sigma of 0.005
 C1_$3, C2_$3, C7_$3, C6_$3, C5_$3, C4_$3, C3_$3, C8_$3, C11_$2, C13_$2
 with sigma of 0.005
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:
 C10(H10A,H10B,H10C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
7.c Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C2)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              22069
_shelx_hkl_checksum              58411
_shelx_fab_checksum              98085
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 319.767
_oxdiff_exptl_absorpt_empirical_full_min 0.535