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_1559688
_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)'
_chemical_formula_sum            'C16 H6 Cd N2 O12'
_chemical_formula_weight         530.63
_chemical_name_common            SHF-81-DMF
_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             2020-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   14.9210(5)
_cell_length_b                   14.9210(5)
_cell_length_c                   12.7118(5)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      66.51
_cell_measurement_theta_min      3.42
_cell_volume                     2450.94(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.705
_diffrn_reflns_theta_max         66.705
_diffrn_reflns_theta_min         3.420
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.745
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1234 before and 0.0819 after correction. The Ratio of minimum to maximum transmission is 0.4906.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1082 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.066(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2901
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0686P)^2^+1.3020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2549
_reflns_number_total             2901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00089b2.cif
_cod_data_source_block           ilb3557_tmr_sq
_cod_depositor_comments
'Adding full bibliography for 1559676--1559688.cif.'
_cod_original_cell_volume        2450.94(19)
_cod_database_code               1559688
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.517(10)
 0.483(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N1-C7
 1.336 with sigma of 0.01
 N1-O6
 1.251 with sigma of 0.01
 C5-C8
 1.4 with sigma of 0.02
 C8-O3
 1.25 with sigma of 0.02
 O4-C8
 1.25 with sigma of 0.02
 O3-O4
 2.25 with sigma of 0.02
4. Restrained planarity
 N1, C7, C2, C6
 with sigma of 0.1
 O5, N1, O6, C7
 with sigma of 0.1
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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4)
6.b Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4)
;
_shelx_res_checksum              89707
_shelx_fab_checksum              23841
_olex2_submission_special_instructions 'No special instructions were received'