A nanoporous 3D zinc(II) metal‒organic framework for selective absorption of benzaldehyde and formaldehyde
Moradpour, Tahereh; Abbasi, Alireza; Van Hecke, Kristof; Journal of Solid State Chemistry 228 (2015) 36–41; doi:10.1016/j.jssc.2015.04.013

data_1561869
_publ_section_title
;
 A nanoporous 3D zinc(II) metal--organic framework for selective
 absorption of benzaldehyde and formaldehyde
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              36
_journal_page_last               41
_journal_paper_doi               10.1016/j.jssc.2015.04.013
_journal_volume                  228
_journal_year                    2015
_chemical_formula_moiety         'C48 H30 N12 O15 Zn4, C3 H7 N O, 6(O)'
_chemical_formula_sum            'C51 H37 N13 O22 Zn4'
_chemical_formula_weight         1445.50
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.836(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.0338(8)
_cell_length_b                   26.3415(7)
_cell_length_c                   27.5327(7)
_cell_measurement_reflns_used    8803
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3660
_cell_measurement_theta_min      3.7090
_cell_volume                     18704.8(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_details
;
  1 omega  -70.00   16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048   95.0000 -154.0000 86

  2 omega  -83.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   95.0000   84.0000 75

  3 omega  102.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   95.0000   25.0000 55

  4 omega  107.00  135.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   95.0000   84.0000 28

  5 omega   50.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -95.0000   95.0000 45

  6 omega   28.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -95.0000  154.0000 81

  7 omega   69.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8048 -125.0000  -90.0000 25

  8 omega -122.00  -80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  -30.0000 42

  9 omega -112.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  120.0000 25

 10 omega   34.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000  150.0000 42

 11 omega   58.00  138.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -61.0000  -60.0000 80

 12 omega   46.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   60.0000 26

 13 omega   29.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -94.0000  -60.0000 71

 14 omega   36.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   30.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0332782000
_diffrn_orient_matrix_UB_12      0.0476111000
_diffrn_orient_matrix_UB_13      0.0050179000
_diffrn_orient_matrix_UB_21      -0.0470000000
_diffrn_orient_matrix_UB_22      -0.0265241000
_diffrn_orient_matrix_UB_23      -0.0294631000
_diffrn_orient_matrix_UB_31      -0.0157706000
_diffrn_orient_matrix_UB_32      -0.0212135000
_diffrn_orient_matrix_UB_33      0.0479584000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17701
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5840
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         17701
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1195P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                11914
_reflns_number_total             17701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-228-36.cif
_cod_data_source_block           final
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1561869
_chemical_oxdiff_formula         'C24 H15 N6 O6 Zn1'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
 N13 \\sim C49 \\sim C50 \\sim C51 \\sim O14: within 1.7A with sigma of 0.01 
 and sigma for terminal atoms of 0.02
 Uanis(N13) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
 \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal 
 atoms of 0.02
 Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
 Uanis(O25) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
 Uanis(O26) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
 Uanis(O29) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
 Uanis(O32) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
 Uanis(O33) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C18(H18), C19(H19), C21(H21), C22(H22), C26(H26), C27(H27), C29(H29), C30(H30),
 C33(H33), C34(H34), C36(H36), C37(H37), C43(H43), C44(H44), C46(H46),
 C47(H47), C51(H51), N1(H1), N4(H4A), N5(H5), N6(H6A), N7(H7A), N11(H11A)
3.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;