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_7228466
_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, 0.57(C3 H7 N O)'
_chemical_formula_sum            'C27.69 H24.94 Cd N4.57 O6.57'
_chemical_formula_weight         639.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                101.807(2)
_cell_angle_beta                 100.473(2)
_cell_angle_gamma                109.366(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2700(10)
_cell_length_b                   10.9495(11)
_cell_length_c                   13.9134(13)
_cell_measurement_reflns_used    6876
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      27.064
_cell_measurement_theta_min      3.000
_cell_volume                     1391.0(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      298.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17445
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.849
_diffrn_reflns_theta_min         1.553
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0180 after correction.
The Ratio of minimum to maximum transmission is 0.8516.
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    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             647
_exptl_crystal_size_max          1.22
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         8571
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8132
_reflns_number_total             8571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00715a2.cif
_cod_data_source_block           298k
_cod_database_code               7228466
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1S1 \\sim N1S1 \\sim C1S1 \\sim C2S1 \\sim C3S1: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C2S1, N1S1, C3S1, O1S1
 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} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1B, C2B, C3B, C4B, C5B}
5. Others
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=
 Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C8B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=
 Sof(H12B)=Sof(N2B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C9B)=Sof(H9B)=Sof(C10B)=
 Sof(H10B)=Sof(N1B)=1-FVAR(1)
 Sof(N2A)=Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=FVAR(1)
 Sof(O1S1)=Sof(N1S1)=Sof(C1S1)=Sof(H1S1)=Sof(C2S1)=Sof(H2SA)=Sof(H2SB)=
 Sof(H2SC)=Sof(C3S1)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=FVAR(2)
6.a Free rotating group:
 O1S1(N1S1,N2A,N1A,C1A,C2A,C3A,C4A,C5A,C7A,C8A,C9A,C10A,C11A,C12A,C1S1,C2S1,
 C3S1,N1C,C1C,C2C,C3C,C4C,C5C,C6C,O1D,O2D,O3D,O4D,O5D,O6D,N1D,C1D,C2D,C3D,C4D,
 C5D,C6D,C7D,C8D,C6B,C1B,C2B,C3B,C4B,C5B,C6A,C8B,C11B,C12B,N2B,C7B,C9B,C10B,N1B)
6.b Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C6C(H6CA,H6CB), C6B(H6BA,H6BB), C6A(H6AA,H6AB), C7B(H7BA,H7BB)
6.c Me refined with riding coordinates:
 C3S1(H3SA,H3SB,H3SC)
6.d Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C1S1(H1S1), C1C(H1C), C2C(H2C), C4C(H4C), C5C(H5C), C2D(H2D),
 C4D(H4D), C6D(H6D), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B), C11B(H11B),
 C12B(H12B), C9B(H9B), C10B(H10B)
6.e Idealised Me refined as rotating group:
 C2S1(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              98529
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'