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_7228464
_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, 0.62(C3 H7 N O)'
_chemical_formula_sum            'C27.86 H25.34 Cd N4.62 O6.62'
_chemical_formula_weight         643.19
_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                100.7670(10)
_cell_angle_beta                 102.2560(10)
_cell_angle_gamma                108.8430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2340(5)
_cell_length_b                   10.8368(6)
_cell_length_c                   13.8265(7)
_cell_measurement_reflns_used    6876
_cell_measurement_temperature    104.15
_cell_measurement_theta_max      27.064
_cell_measurement_theta_min      3.000
_cell_volume                     1363.02(12)
_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      104.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_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       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17010
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.655
_diffrn_reflns_theta_min         1.568
_exptl_absorpt_coefficient_mu    0.854
_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    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          1.22
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.33
_refine_diff_density_max         2.626
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_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^+2.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8177
_reflns_number_total             8338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00715a2.cif
_cod_data_source_block           104k
_cod_database_code               7228464
_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
N2A \\sim C10A \\sim C9A \\sim C8A \\sim C12A \\sim C11A \\sim N2B \\sim C10B
\\sim C9B \\sim C8B \\sim C12B \\sim C11B \\sim C6A \\sim C7A \\sim C6B \\sim
C7B \\sim C2A \\sim C3A \\sim C4A \\sim C2B \\sim C3B \\sim C4B \\sim N1A \\sim
C1A \\sim C5A \\sim N1B \\sim C1B \\sim C5B: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 O1S1, N1S1, C1S1, C2S1, C3S1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7A, N2A, C10A, C9A, C8A, C12A, C11A, C7B, N2B, C10B, C9B, C8B, C12B, C11B,
 C3A, C6A, C3B, C6B, N1A, C1A, C2A, C4A, C5A, N1B, C1B, C2B, C4B, C5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{N1A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N2A, C10A, C9A, C8A, C12A, C11A}
{N1B, C1B, C2B, C3B, C4B, C5B} sigma for 1-2: 0.02, 1-3: 0.04
as
{N2B, C10B, C9B, C8B, C12B, C11B}
5. Others
 Sof(N1B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=
 Sof(N2B)=Sof(C10B)=Sof(H10B)=Sof(C9B)=Sof(H9B)=Sof(C8B)=Sof(C12B)=Sof(H12B)=
 Sof(C11B)=Sof(H11B)=1-FVAR(1)
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(N2A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(C12A)=Sof(H12A)=
 Sof(C11A)=Sof(H11A)=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,C1S1,C2S1,C3S1,N1B,C1B,C2B,C3B,C4B,C5B,C6B,C7B,N2B,C10B,C9B,C8B,
 C12B,C11B)
6.b Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C7A(H7AA,H7AB), C6C(H6CA,H6CB), C6B(H6BA,H6BB), 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), C10A(H10A), C9A(H9A), C12A(H12A),
 C11A(H11A), C1C(H1C), C2C(H2C), C4C(H4C), C5C(H5C), C2D(H2D), C4D(H4D),
 C6D(H6D), C1S1(H1S1), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B), C10B(H10B),
 C9B(H9B), C12B(H12B), C11B(H11B)
6.e Idealised Me refined as rotating group:
 C2S1(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              30647
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'