Metal-organic frameworks as stationary phases for mixed-mode separation applications
Turner, David R.; Hawes, Chris S.; Batten, Stuart R.; Knowles, Gregory P.; Chaffee, Alan L.; Nolvachai, Yada; Kulsing, Chadin; Marriott, Philip J.; Chem.Commun. 50 (2014) 3735–; doi:10.1039/C4CC00933A

data_7112164
_publ_section_title
;
 Metal-organic frameworks as stationary phases for mixed-mode separation
 applications
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_journal_name_full               Chem.Commun.
_journal_page_first              3735
_journal_paper_doi               10.1039/C4CC00933A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '0.25(C160 H160 Cd8 N16 O32)'
_chemical_formula_sum            'C40 H40 Cd2 N4 O8'
_chemical_formula_weight         929.56
_chemical_name_systematic        ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.722(4)
_cell_length_b                   39.084(8)
_cell_length_c                   17.966(4)
_cell_measurement_temperature    273
_cell_volume                     15253(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28405
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details          '8 H2O, 5.5 DMF per Cd2, bulk dry material'
_refine_diff_density_max         1.738
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2524
_reflns_number_gt                5513
_reflns_number_total             8251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00933a2.cif
_cod_data_source_block           1B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-Scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7112164
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C22-H22B
 0.97 with sigma of 0.02
 H22A-C22
 0.97 with sigma of 0.02
 H32-C32
 0.97 with sigma of 0.02
 H15-C15
 0.97 with sigma of 0.02
 C37-O38
 1.25 with sigma of 0.02
 C37-O39
 1.25 with sigma of 0.02
 O39-O38
 0.8 with sigma of 0.02
 H15-H15_$1
 1.5 with sigma of 0.04
 H32-H32_$1
 1.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: N3(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 N6(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) N9(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) N12(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) O38(0.5) O39(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C24(H24), C25(H25), C27(H27), C28(H28), C34(H34), C35(H35)
;