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_1559682
_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             2020-05-26
_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                   13.6191(13)
_cell_length_b                   13.6191(13)
_cell_length_c                   13.2288(13)
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.680
_cell_measurement_theta_min      3.341
_cell_volume                     2124.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 1.000
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            71934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.675
_diffrn_reflns_theta_max         66.675
_diffrn_reflns_theta_min         3.341
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.728
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0985 before and 0.0788 after correction. The Ratio of minimum to maximum transmission is 0.7602. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             942
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.123
_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   0.031(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2516
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0617P)^2^+9.5605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2507
_reflns_number_total             2516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00089b2.cif
_cod_data_source_block           ilb3559_tmr-r_0m
_cod_depositor_comments
'Adding full bibliography for 1559676--1559688.cif.'
_cod_original_cell_volume        2124.9(5)
_cod_database_code               1559682
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.196
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.497(4)
 0.503(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. Restrained distances
 C8B-O
 1.2 with sigma of 0.02
 C8A-O7AA
 1.2 with sigma of 0.02
 C8A-O6AA
 1.2 with sigma of 0.02
 O7AA-O6AA
 2.03 with sigma of 0.02
 C8B-O9AA
 1.2 with sigma of 0.02
 O9AA-O
 2 with sigma of 0.02
 C8B-C5B
 1.5 with sigma of 0.02
 O8AA-O4AA
 2.2 with sigma of 0.02
 O8AA-N0AA
 1.22 with sigma of 0.02
 N0AA-O4AA
 1.22 with sigma of 0.02
 C4A-O8AA
 2.3 with sigma of 0.02
 O5AA-O3AA
 2.2 with sigma of 0.02
 O5AA-N1AA
 1.22 with sigma of 0.02
 N1AA-O3AA
 1.22 with sigma of 0.02
 C10B-C9B
 2.3 with sigma of 0.02
 N2AA-C10B
 1.3 with sigma of 0.02
 N2AA-C9B
 1.3 with sigma of 0.02
 C10A-C9A
 2.3 with sigma of 0.02
 C9A-N
 1.3 with sigma of 0.02
 N-C10A
 1.3 with sigma of 0.02
4. Restrained planarity
 C1, C3A, C4A, C8A, N1AA, C2B, C5B, C6B, C7B
 with sigma of 0.1
5. Rigid bond restraints
 O6AA, O7AA, C8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2AA, C1, O0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3AA, O5AA, N1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O6AA \\sim O7AA \\sim C8A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O2AA \\sim C1 \\sim O0AA: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O3AA \\sim O5AA \\sim N1AA: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
7. 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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(O9AA)=Sof(O)=Sof(O3AA)=Sof(O5AA)=Sof(N1AA)=Sof(C2B)=Sof(C3B)=Sof(H3B)=
 Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=1-FVAR(1)
 Sof(O6AA)=Sof(O7AA)=Sof(O4AA)=Sof(O8AA)=Sof(N0AA)=Sof(C5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C8A)=FVAR(1)
 Sof(O1AA)=1-FVAR(2)
 Sof(O0AA)=FVAR(2)
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(H9BC)=Sof(N2AA)=Sof(H2AA)=Sof(H2AB)=1-FVAR(3)
 Sof(N)=Sof(HA)=Sof(HB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
9.a Secondary CH2 refined with riding coordinates:
 N(HA,HB), N2AA(H2AA,H2AB)
9.b Me refined with riding coordinates:
 C9A(H9AA,H9AB,H9AC), C10B(H10D,H10E,H10F), C10A(H10A,H10B,H10C), C9B(H9BA,
 H9BB,H9BC)
9.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C7A(H7A), C3A(H3A), C3B(H3B), C6B(H6B), C7B(H7B)
9.d Fitted hexagon refined as free rotating group:
 C5A(C6A,C7A,C2A,C3A,C4A), C2B(C3B,C4B,C5B,C6B,C7B)
;
_shelx_res_checksum              21169
_olex2_submission_special_instructions 'No special instructions were received'