#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:21:51 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261707 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/96/1559687.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559687
loop_
_publ_author_name
'Watkins, Daniel'
'Roseveare, Thomas M.'
'Warren, Mark R.'
'Thompson, Stephen P.'
'Fletcher, Ashleigh J.'
'Brammer, Lee'
_publ_section_title
;
 Multi-stimulus linear negative expansion of a breathing
 M(O₂CR)₄-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                   14.8744(10)
_cell_length_b                   14.8744(10)
_cell_length_c                   12.7248(9)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.55
_cell_measurement_theta_min      3.43
_cell_volume                     2438.2(3)
_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      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32861
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.660
_diffrn_reflns_theta_max         66.660
_diffrn_reflns_theta_min         3.431
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.775
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1281 before and 0.0844 after correction. The Ratio of minimum to maximum transmission is 0.4774.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.084
_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         0.384
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1069 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.074(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2877
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0335
_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/[σ²(Fo²)+(0.0608P)²+2.1129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2518
_reflns_number_total             2877
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0fd00089b2.cif
_cod_data_source_block           ilb3558_tmr_sq
_cod_depositor_comments
'Adding full bibliography for 1559676--1559688.cif.'
_cod_original_cell_volume        2438.1(4)
_cod_database_code               1559687
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.514(10)
 0.486(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O7-O2
 2.25 with sigma of 0.02
 O2-C7
 1.25 with sigma of 0.02
 O7-C7
 1.25 with sigma of 0.02
 C7-C6
 1.4 with sigma of 0.02
4. Restrained planarity
 N6, C0AA, C4, C8
 with sigma of 0.1
 O11, N6, O13, C0AA
 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:
 C17(H17), C8(H8), C19(H19)
6.b Fitted hexagon refined as free rotating group:
 C17(C4,C0AA,C8,C6,C19)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.49969(15) -0.49969(15) 0.000000 0.0429(2) Uani 1 2 d S TU P . .
C5 C -0.4980(14) -0.3683(12) -0.1557(13) 0.067(4) Uani 1 1 d . U . . .
O0AA O -0.5898(12) -0.4402(12) -0.1183(12) 0.090(4) Uani 1 1 d . U . . .
C17 C -0.5958(6) -0.3300(11) -0.2921(13) 0.076(5) Uani 1 1 d . U . . .
H17 H -0.658658 -0.386364 -0.266233 0.091 Uiso 1 1 calc R . . . .
C4 C -0.5023(10) -0.3027(12) -0.2425(10) 0.075(4) Uani 1 1 d G U . . .
C0AA C -0.4103(6) -0.2202(13) -0.2804(12) 0.113(6) Uani 1 1 d G U . . .
C8 C -0.4117(7) -0.1650(11) -0.3679(12) 0.104(6) Uani 1 1 d G U . . .
H8 H -0.348764 -0.108671 -0.393761 0.124 Uiso 1 1 calc R . . . .
C6 C -0.5051(10) -0.1923(11) -0.4175(9) 0.075(4) Uani 1 1 d DG U . . .
C19 C -0.5972(6) -0.2748(12) -0.3796(12) 0.071(4) Uani 1 1 d G U . . .
H19 H -0.661048 -0.293421 -0.413552 0.085 Uiso 1 1 calc R . . . .
O1 O -0.4219(13) -0.3532(13) -0.1127(11) 0.115(6) Uani 1 1 d . U . . .
O2 O -0.4264(12) -0.0733(9) -0.5567(11) 0.092(4) Uani 1 1 d D U . . .
C7 C -0.5146(14) -0.1347(16) -0.5145(15) 0.080(6) Uani 1 1 d D U . . .
O7 O -0.5935(12) -0.1381(13) -0.5341(12) 0.096(5) Uani 1 1 d D U . . .
N6 N -0.3165(17) -0.1772(15) -0.2348(16) 0.150(7) Uani 1 1 d . U . . .
O11 O -0.246(3) -0.182(3) -0.276(2) 0.342(18) Uani 1 1 d . U . . .
O13 O -0.300(3) -0.134(3) -0.142(3) 0.36(2) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O0AA Cd1 O0AA 169.4(7) 6 . ?
O0AA Cd1 C7 92.2(6) 6 3_445 ?
O0AA Cd1 C7 84.8(6) . 3_445 ?
O0AA Cd1 C7 84.8(6) 6 5_444 ?
O0AA Cd1 C7 92.2(6) . 5_444 ?
O0AA Cd1 O7 82.4(3) . 3_445 ?
O0AA Cd1 O7 99.2(3) . 5_444 ?
O0AA Cd1 O7 99.2(3) 6 3_445 ?
O0AA Cd1 O7 82.4(3) 6 5_444 ?
O1 Cd1 O0AA 53.3(5) . . ?
O1 Cd1 O0AA 53.3(5) 6 6 ?
O1 Cd1 O0AA 136.8(6) . 6 ?
O1 Cd1 O0AA 136.8(6) 6 . ?
O1 Cd1 O1 90.6(8) . 6 ?
O1 Cd1 C7 90.7(7) . 5_444 ?
O1 Cd1 C7 113.4(6) . 3_445 ?
O1 Cd1 C7 90.7(7) 6 3_445 ?
O1 Cd1 C7 113.4(6) 6 5_444 ?
O1 Cd1 O7 75.8(5) 6 3_445 ?
O1 Cd1 O7 92.4(6) . 3_445 ?
O1 Cd1 O7 75.7(5) . 5_444 ?
O1 Cd1 O7 92.4(6) 6 5_444 ?
O2 Cd1 O0AA 89.1(5) 5_444 6 ?
O2 Cd1 O0AA 89.1(5) 3_445 . ?
O2 Cd1 O0AA 83.4(5) 5_444 . ?
O2 Cd1 O0AA 83.4(5) 3_445 6 ?
O2 Cd1 O1 106.3(3) 3_445 6 ?
O2 Cd1 O1 106.3(3) 5_444 . ?
O2 Cd1 O1 134.5(4) 5_444 6 ?
O2 Cd1 O1 134.5(4) 3_445 . ?
O2 Cd1 O2 91.5(7) 5_444 3_445 ?
O2 Cd1 C7 118.4(7) 5_444 3_445 ?
O2 Cd1 C7 28.2(4) 3_445 3_445 ?
O2 Cd1 C7 28.2(4) 5_444 5_444 ?
O2 Cd1 C7 118.4(7) 3_445 5_444 ?
O2 Cd1 O7 53.8(4) 3_445 3_445 ?
O2 Cd1 O7 142.5(5) 3_445 5_444 ?
O2 Cd1 O7 53.8(4) 5_444 5_444 ?
O2 Cd1 O7 142.5(5) 5_444 3_445 ?
C7 Cd1 C7 146.2(8) 5_444 3_445 ?
O7 Cd1 C7 170.3(6) 5_444 3_445 ?
O7 Cd1 C7 25.6(4) 3_445 3_445 ?
O7 Cd1 C7 170.3(6) 3_445 5_444 ?
O7 Cd1 C7 25.6(4) 5_444 5_444 ?
O7 Cd1 O7 163.3(7) 3_445 5_444 ?
O0AA C5 C4 115.3(14) . . ?
O1 C5 O0AA 119.4(14) . . ?
O1 C5 C4 124.8(17) . . ?
C5 O0AA Cd1 89.0(10) . . ?
C4 C17 C19 120.0 . . ?
C17 C4 C5 120.5(12) . . ?
C0AA C4 C5 119.2(12) . . ?
C0AA C4 C17 120.0 . . ?
C4 C0AA C8 120.0 . . ?
N6 C0AA C4 127.0(13) . . ?
N6 C0AA C8 112.6(13) . . ?
C0AA C8 C6 120.0 . . ?
C8 C6 C7 123.7(12) . . ?
C19 C6 C8 120.0 . . ?
C19 C6 C7 116.3(12) . . ?
C6 C19 C17 120.0 . . ?
C5 O1 Cd1 97.2(12) . . ?
C7 O2 Cd1 91.8(11) . 2_454 ?
C6 C7 Cd1 168.7(12) . 2_454 ?
O2 C7 Cd1 60.1(9) . 2_454 ?
O2 C7 C6 112.6(15) . . ?
O7 C7 Cd1 65.7(11) . 2_454 ?
O7 C7 C6 120.7(16) . . ?
O7 C7 O2 125.8(17) . . ?
C7 O7 Cd1 88.6(12) . 2_454 ?
O11 N6 C0AA 121(3) . . ?
O11 N6 O13 118(3) . . ?
O13 N6 C0AA 121(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O0AA 2.456(12) 6 ?
Cd1 O0AA 2.456(12) . ?
Cd1 O1 2.371(13) . ?
Cd1 O1 2.371(13) 6 ?
Cd1 O2 2.356(13) 5_444 ?
Cd1 O2 2.356(13) 3_445 ?
Cd1 C7 2.718(17) 3_445 ?
Cd1 C7 2.718(17) 5_444 ?
Cd1 O7 2.478(15) 5_444 ?
Cd1 O7 2.478(15) 3_445 ?
C5 O0AA 1.33(2) . ?
C5 C4 1.496(15) . ?
C5 O1 1.17(2) . ?
C17 C4 1.3900 . ?
C17 C19 1.3900 . ?
C4 C0AA 1.3900 . ?
C0AA C8 1.3900 . ?
C0AA N6 1.34(2) . ?
C8 C6 1.3900 . ?
C6 C19 1.3900 . ?
C6 C7 1.548(17) . ?
O2 C7 1.283(17) . ?
C7 O7 1.176(16) . ?
N6 O11 1.21(3) . ?
N6 O13 1.31(3) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.514(10)
2 0.486(10)
