A Cd mixed-ligand MOF showing Ligand-Disorder Induced Breathing Behaviour at High Temperature and Stepwise, Selective Carbon Dioxide Adsorption at Low Temperature
Tahier, Tayyibah; Oliver, Clive L.; CrystEngComm  (2017) –; doi:10.1039/C7CE00715A

data_7228467
_publ_section_title
;
 A Cd mixed-ligand MOF showing Ligand-Disorder Induced Breathing Behaviour
 at High Temperature and Stepwise, Selective Carbon Dioxide Adsorption at
 Low Temperature
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00715A
_journal_year                    2017
_chemical_formula_moiety         'C26 H21 Cd N4 O6'
_chemical_formula_sum            'C26 H21 Cd N4 O6'
_chemical_formula_weight         597.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-12 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.635(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.330(6)
_cell_length_b                   10.234(2)
_cell_length_c                   20.922(5)
_cell_measurement_reflns_used    6876
_cell_measurement_temperature    373.15
_cell_measurement_theta_max      27.064
_cell_measurement_theta_min      3.000
_cell_volume                     5476(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      373.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23205
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.643
_diffrn_reflns_theta_min         1.592
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1047 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.6468.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          1.22
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.527
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8102
_refine_ls_number_restraints     1080
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+6.9837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4524
_reflns_number_total             8102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00715a2.cif
_cod_data_source_block           373k
_cod_database_code               7228467
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C1B
\\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim N1C \\sim C1C \\sim C2C
\\sim C3C \\sim C4C \\sim C5C \\sim C6C \\sim O3D \\sim O1E \\sim O2E \\sim O4E
\\sim O5E \\sim O6E \\sim N1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E
\\sim C6E \\sim C7E \\sim C8D \\sim C6A \\sim C2D \\sim C2A \\sim O5D \\sim C6D
\\sim C4A \\sim O2D \\sim N1D \\sim C4D \\sim C8E \\sim C1A \\sim C3A \\sim C5A
\\sim O1D \\sim O4D \\sim O6D \\sim C1D \\sim C3D \\sim C5D \\sim C7D: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 N1, N2, C7, C8, C9, C10, C11, C12, C1B, C2B, C3B, C4B, C5B, C6B, N1C, C1C,
 C2C, C3C, C4C, C5C, C6C, O3D, O1E, O2E, O4E, O5E, O6E, N1E, C1E, C2E, C3E, C4E,
  C5E, C6E, C7E, C8D, C6A, C2D, C2A, O5D, C6D, C4A, O2D, N1D, C4D, C8E, C1A,
 C3A, C5A, O1D, O4D, O6D, C1D, C3D, C5D, C7D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1B, C2B, C3B, C4B, C5B, C6B}
{O1D, O2D} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1E, O2E}
{O4D, O5D, O6D, N1D, C1D, C2D, C3D, C4D, C5D, C6D, C7D, C8E} sigma for 1-2:
0.02, 1-3: 0.04
as
{O4E, O5E, O6E, N1E, C1E, C2E, C3E, C4E, C5E, C6E, C7E, C8D}
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=
 Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=FVAR(1)
 Sof(O1E)=Sof(O2E)=Sof(O4E)=Sof(O5E)=Sof(O6E)=Sof(N1E)=Sof(C1E)=Sof(C2E)=
 Sof(H2E)=Sof(C3E)=Sof(C4E)=Sof(H4E)=Sof(C5E)=Sof(C6E)=Sof(H6E)=Sof(C7E)=
 Sof(C8E)=1-FVAR(2)
 Sof(C8D)=Sof(O4D)=Sof(O5D)=Sof(O6D)=Sof(N1D)=Sof(C1D)=Sof(C2D)=Sof(H2D)=
 Sof(C3D)=Sof(C4D)=Sof(H4D)=Sof(C5D)=Sof(C6D)=Sof(H6D)=Sof(C7D)=Sof(O1D)=
 Sof(O2D)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7BC,H7BD), C7(H7AA,H7AB), C6B(H6BA,H6BB), C6C(H6CA,H6CB), C6A(H6AA,H6AB)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B),
 C1C(H1C), C2C(H2C), C4C(H4C), C5C(H5C), C2E(H2E), C4E(H4E), C6E(H6E), C1A(H1A),
  C2A(H2A), C4A(H4A), C5A(H5A), C2D(H2D), C4D(H4D), C6D(H6D)
;
_shelx_res_checksum              59067
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'