Multi-stimulus linear negative expansion of a breathing M(O<sub>2</sub>CR)<sub>4</sub>-node MOF.
Watkins, Daniel; Roseveare, Thomas M.; Warren, Mark R.; Thompson, Stephen P.; Fletcher, Ashleigh J.; Brammer, Lee; Faraday discussions 225 (2021) 133–151; doi:10.1039/d0fd00089b

data_1559677
_publ_section_title
;
 Multi-stimulus linear negative expansion of a breathing
 M(O<sub>2</sub>CR)<sub>4</sub>-node MOF.
;
_journal_name_full               'Faraday discussions'
_journal_page_first              133
_journal_page_last               151
_journal_paper_doi               10.1039/d0fd00089b
_journal_volume                  225
_journal_year                    2021
_chemical_formula_moiety         '0.33(C48 H18 Cd3 N6 O36), 2(C2 H8 N)'
_chemical_formula_sum            'C20 H22 Cd N4 O12'
_chemical_formula_weight         622.81
_chemical_name_common            SHF-81
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.9775(9)
_cell_length_b                   13.9775(9)
_cell_length_c                   13.0994(5)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.2030
_cell_measurement_theta_min      1.6270
_cell_volume                     2216.4(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
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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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -92.00   38.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   45.0000  -80.0000 325

  2 phi    -80.00   40.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000   45.0000     -     300

  3 omega  -92.00   38.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   45.0000   40.0000 325

  4 phi     40.00  160.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000   45.0000     -     300

  5 omega  -92.00   38.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   45.0000  160.0000 325

  6 phi    -90.00  150.00   0.4000    0.1970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000    0.0000     -     600
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      0.0095903000
_diffrn_orient_matrix_UB_12      0.0353978000
_diffrn_orient_matrix_UB_13      -0.0402301000
_diffrn_orient_matrix_UB_21      0.0492373000
_diffrn_orient_matrix_UB_22      0.0016221000
_diffrn_orient_matrix_UB_23      -0.0098814000
_diffrn_orient_matrix_UB_31      -0.0268983000
_diffrn_orient_matrix_UB_32      -0.0445035000
_diffrn_orient_matrix_UB_33      -0.0323735000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31828
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.946
_diffrn_reflns_theta_min         1.507
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       needle
_exptl_crystal_F_000             942
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1230P)^2^+0.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.2159
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2514
_reflns_number_total             4713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00089b2.cif
_cod_data_source_block           1barco2_rt_2_
_cod_depositor_comments
'Adding full bibliography for 1559676--1559688.cif.'
_cod_original_cell_volume        2216.4(3)
_cod_database_code               1559677
_chemical_oxdiff_formula         'Cd O12 N4 C20 H22'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.95
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.512(4) 0.488(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. 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
4.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4)
4.c Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4)
4.d Idealised Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              75153
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'