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_4131850
_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             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3348(12)
_cell_length_b                   19.3348(12)
_cell_length_c                   32.768(5)
_cell_measurement_reflns_used    2218
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.2320
_cell_measurement_theta_min      2.0720
_cell_volume                     12250(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 Dectris
_diffrn_detector_area_resol_mean 5.81395
_diffrn_detector_type            'Pilatus 300K detector'
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_diffrn_measurement_details
;
  1 omega -105.00  -74.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -       20.0000   70.0000  155.7700 155

  2 omega -105.00  -74.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -       20.0000   70.0000  -24.2300 155

  3 omega -106.00  -66.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -70.0000 -155.7700 200

  4 omega -106.00  -66.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -70.0000   24.2300 200

  5 omega -150.00  -94.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -      -20.0000   70.0000  -24.2319 280

  6 omega -150.00  -94.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -      -20.0000   70.0000  155.7681 280

  7 omega  -96.00  -30.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -70.0000   24.2300 330

  8 omega  -96.00  -30.00   0.2000    0.9970
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -70.0000 -155.7700 330
;
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type
'Newport 4-circle kappa geometry diffractometer'
_diffrn_measurement_method       'oscillation method'
_diffrn_orient_matrix_UB_11      0.0012960000
_diffrn_orient_matrix_UB_12      -0.0317471000
_diffrn_orient_matrix_UB_13      -0.0094373000
_diffrn_orient_matrix_UB_21      -0.0160321000
_diffrn_orient_matrix_UB_22      0.0138042000
_diffrn_orient_matrix_UB_23      -0.0169514000
_diffrn_orient_matrix_UB_31      0.0318118000
_diffrn_orient_matrix_UB_32      0.0081679000
_diffrn_orient_matrix_UB_33      -0.0081593000
_diffrn_radiation_collimation    '0.5 mm pinhole'
_diffrn_radiation_monochromator  'Si 111 double-crystal monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.8004
_diffrn_reflns_av_unetI/netI     0.6238
_diffrn_reflns_Laue_measured_fraction_full 0.765
_diffrn_reflns_Laue_measured_fraction_max 0.765
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24054
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.765
_diffrn_reflns_theta_full        22.719
_diffrn_reflns_theta_max         22.719
_diffrn_reflns_theta_min         1.880
_diffrn_source                   'Synchrotron U21 undulator'
_diffrn_source_type              'Synchrotron Diamond Light Source'
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.4269
_exptl_absorpt_correction_T_min  0.2358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.1745 before and 0.1272 after correction. 
The Ratio of minimum to maximum transmission is 0.5524. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.605
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.0806
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         3547
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.3788
_refine_ls_R_factor_gt           0.2144
_refine_ls_shift/su_max          0.000
_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          0.4531
_refine_ls_wR_factor_ref         0.5525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1058
_reflns_number_total             3547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZrMOF_All.cif
_cod_data_source_block           14.9kbar
_cod_database_code               4131850
_chemical_oxdiff_formula         'C46 H42 O16 Zr3'
_reflns_odcompleteness_completeness 74.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.88
_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
 C2-C7 = C3-C2 = C4-C3 = C4-C5 = C6-C5 = C7-C6
 1.39 with sigma of 0.01
 C8-C9 = C8-C11 = C12-C11
 1.39 with sigma of 0.01
 C2-C1
 1.5 with sigma of 0.02
 C10-C9
 1.5 with sigma of 0.02
 C8-C5
 1.5 with sigma of 0.01
 C12-C12_$2
 1.5 with sigma of 0.01
 C13-C11
 1.5 with sigma of 0.01
 C4-C5 \\sim C2-C7 \\sim C3-C2 \\sim C4-C3 \\sim C6-C5 \\sim C7-C6
 with sigma of 0.02
3. Restrained planarity
 C2_$1, C3_$1, C4_$1, C5_$1, C6_$1, C7_$1, C8_$1, C11, C13, C1_$1
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6, C7, C8, C11_$1
 with sigma of 0.1
 C1_$2, C2_$2, C7_$2, C6_$2, C5_$2, C4_$2, C3_$2, C8_$2, C11_$3, C13_$3
 with sigma of 0.1
 C1_$3, C3_$3, C4_$3, C5_$3, C6_$3, C7_$3, C2_$3, C8_$3, C11_$2, C13_$2
 with sigma of 0.1
 C10, C9, C12, C12_$2, C9_$2, C10_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
5. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5)
6.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              48844
_shelx_hkl_checksum              91470
_shelx_fab_checksum              2335
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'