An anionic metal‒organic framework: metathesis of zinc(ii) with copper(ii) for efficient C3/C2 hydrocarbon and organic dye separation
Liu, Xiuping; Hao, Chunlian; Li, Jing; Wang, Yutong; Hou, Yongchun; Li, Xue; Zhao, Lianming; Zhu, Houyu; Guo, Wenyue; Inorganic Chemistry Frontiers 5 (2018) 2898–; doi:10.1039/C8QI00773J

data_4349907
_publ_section_title
;
 An anionic metal--organic framework: metathesis of zinc(ii) with
 copper(ii) for efficient C3/C2 hydrocarbon and organic dye separation
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2898
_journal_paper_doi               10.1039/C8QI00773J
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C31 H30 N4 O13 Zn2'
_chemical_formula_sum            'C31 H30 N4 O13 Zn2'
_chemical_formula_weight         797.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2bc 2'
_space_group_name_H-M_alt        'P 2 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-08 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4950(6)
_cell_length_b                   13.7761(5)
_cell_length_c                   26.8721(8)
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      69.7420
_cell_measurement_theta_min      4.5740
_cell_volume                     4995.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  22.00   1.00    1.00    --    0.00 -57.00 -90.00   27
  2  \w    -65.00 -38.00   1.00    1.00    --    0.00 -57.00 -90.00   27
  3  \w    -30.00   0.00   1.00    1.00    --    0.00  77.00-120.00   30
  4  \w     32.00  68.00   1.00    1.00    --    0.00  77.00-120.00   36
  5  \w     51.00 124.00   1.00    3.96    --   54.00  38.00  60.00   73
  6  \w     72.00 106.00   1.00    3.96    --   54.00 159.00 100.00   34
  7  \w     34.00 116.00   1.00    3.96    --   54.00  77.00 150.00   82
  8  \w    107.00 171.00   1.00    3.96    --  108.00 111.00-120.00   64
  9  \w    100.00 157.00   1.00    3.96    --  108.00  77.00 150.00   57
 10  \w    120.00 176.00   1.00    3.96    --  108.00 111.00 -30.00   56
 11  \w     38.00 131.00   1.00    3.96    --  108.00 -50.00 -60.00   93
 12  \w    101.00 133.00   1.00    3.96    --  108.00 111.00-150.00   32
 13  \w    132.00 175.00   1.00    3.96    --  108.00 111.00  30.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0111345000
_diffrn_orient_matrix_UB_12      -0.0841320000
_diffrn_orient_matrix_UB_13      0.0373850000
_diffrn_orient_matrix_UB_21      0.1124938000
_diffrn_orient_matrix_UB_22      -0.0021381000
_diffrn_orient_matrix_UB_23      -0.0096801000
_diffrn_orient_matrix_UB_31      0.0158314000
_diffrn_orient_matrix_UB_32      0.0736419000
_diffrn_orient_matrix_UB_33      0.0423818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12786
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.876
_diffrn_reflns_theta_min         3.605
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
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    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(8)
_refine_ls_extinction_coef       0.0110(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8157
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.291
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2928
_refine_ls_wR_factor_ref         0.3008
_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_full    0.719
_reflns_Friedel_fraction_max     0.687
_reflns_number_gt                7381
_reflns_number_total             8157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00773j2.cif
_cod_data_source_block           NEM-7-Zn
_cod_database_code               4349907
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zn'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(8)
 0.11(8)
2. 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
3. Shared sites
{C11, N5}
4. Restrained distances
 C30-C31
 2.5 with sigma of 0.02
 O13-O14
 2.2 with sigma of 0.02
 O13-C33 = C33-O14
 1.2 with sigma of 0.02
 C33-C10
 1.4 with sigma of 0.02
 O13-C10 = C10-O14
 2.4 with sigma of 0.02
 C34-C32
 1.4 with sigma of 0.02
 O15-C34 = C34-O16
 1.2 with sigma of 0.02
 O15-O16
 2.2 with sigma of 0.02
 O15-C32 = C32-O16
 2.4 with sigma of 0.02
 H22-H17
 2.2 with sigma of 0.02
 H28C_$1-H28C
 2.2 with sigma of 0.02
 O13-C10 \\sim C10-O14
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C11) = Uanis(N5)
6. Rigid body (RIGU) restrains
 C10, C33, O13, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32, C34, O16, O15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, O15, C34, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, N2, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C21, C22, C32, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C9, C10, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H10(0.5) C11(0.5) H11(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5)
 C32(0.5) N4(0.5) H4(0.5) N5(0.5) H5(0.5) O13(0.5) C33(0.5) O14(0.5) C34(0.5)
 O16(0.5) O15(0.5)
8.a Riding coordinates:
 C11(H11), N4(H4), N5(H5)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C10(H10), C14(H14), C17(H17), C19(H19), C21(H21),
 C22(H22), C23(H23), C26(H26), C29(H29)
8.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              21558
_shelx_hkl_checksum              52467
_shelx_fab_checksum              29964
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.708