Metal nuclearity affects network connectivity: a series of highly connected metal‒organic frameworks based on polynuclear metal clusters as secondary building units
Xu, Yu-Ci; Chen, Yu; Qiu, Hai-Jiang; Zeng, Xiao-Shan; Xu, Hui-Ling; Li, Jie; Zeng, Yong-Fei; Xiao, Dong-Rong; CrystEngComm 18 (2016) 8182–; doi:10.1039/C6CE01287F

data_7236172
_publ_section_title
;
 Metal nuclearity affects network connectivity: a series of highly
 connected metal--organic frameworks based on polynuclear metal clusters
 as secondary building units
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8182
_journal_paper_doi               10.1039/C6CE01287F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 N4 O18 Zn3, C13 H16 N2, H2 O'
_chemical_formula_sum            'C45 H30 N6 O19 Zn3'
_chemical_formula_weight         1154.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-10
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.05.11 svn.r3296 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                112.1787(15)
_cell_angle_beta                 101.8630(14)
_cell_angle_gamma                93.0017(13)
_cell_formula_units_Z            1
_cell_length_a                   9.67809(16)
_cell_length_b                   10.27573(15)
_cell_length_c                   11.9152(2)
_cell_measurement_reflns_used    12393
_cell_measurement_temperature    288.53(10)
_cell_measurement_theta_max      71.3360
_cell_measurement_theta_min      5.4530
_cell_volume                     1062.75(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -32.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000    0.0000 94

  2 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  -30.0000 73

  3 omega   57.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  -30.0000 50

  4 omega  -32.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000   30.0000 94

  5 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  150.0000 73

  6 omega   16.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000 -180.0000 88

  7 omega  -34.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203    0.0000  150.0000 139

  8 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000  -60.0000 84

  9 omega   55.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203 -178.0000  -60.0000 53

 10 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

 11 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 58

 12 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 13 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

 14 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

 15 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 71

 16 omega   70.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 108

 17 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -60.0000 71

 18 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

 19 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

 20 omega   91.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85

 21 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 22 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 23 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 24 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 25 omega   40.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

 26 omega   39.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

 27 omega   38.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -150.0000 78

 28 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   60.0000 95

 29 omega  -34.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -38.0000   90.0000 88

 30 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -120.0000 84

 31 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000 -120.0000 95

 32 omega   16.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000  150.0000 88

 33 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000    0.0000 95

 34 omega   18.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000    0.0000 84

 35 omega    8.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  150.0000 95

 36 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

 37 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91

 38 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

 39 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 91

 40 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 41 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 42 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

 43 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

 44 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

 45 omega   70.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108

 46 omega   87.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -60.0000 91

 47 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 48 omega   81.00  161.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 80

 49 omega   81.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.529
_diffrn_reflns_theta_min         4.696
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0349P)^2^+1.2862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             4100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           4
_cod_database_code               7236172
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C6B-C5A \\sim C6A-C5B \\sim C7-C6B \\sim C7-C6A
 with sigma of 0.02
 C3A-C2A \\sim C3B-C2B \\sim C7-C2A \\sim C7-C2B
 with sigma of 0.02
 C13B-C12 \\sim C14B-C13A \\sim C14A-C13B \\sim C13A-C12
 with sigma of 0.02
 C12-C11B \\sim C12-C11A \\sim C11B-C10B \\sim C11A-C10A
 with sigma of 0.02
3. Restrained planarity
 C7, C2A, C3A, C4A, C5A, C6B
 with sigma of 0.1
 C14A, C9A, C10A, C11A, C12, C13B
 with sigma of 0.1
4. Rigid bond restraints
 N2, N1A, O0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
N2 \\sim N1A \\sim O0AA: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N1A \\sim O0AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C3A \\sim C2A \\sim C7: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
C12 \\sim C13B \\sim C14A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
6. Rigid body (RIGU) restrains
 C29, C18, C19, C17, C20, C22, N3, C21, C23, C24, C25, C26, C28, C27, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6B, H7B, H12A, C13B, N1A, N2, O0AA, C5A, H5A, C4A, C3A, H3A, C2A, C9A, C14A,
 H14A, C10A, H10A, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: C2B(0.65) C3B(0.65) H3B(0.65) C4B(0.65) C5B(0.65) H5B(0.65)
 C6B(0.35) H7A(0.65) H7B(0.35) C9B(0.65) C10B(0.65) H10B(0.65) C11B(0.65)
 H12(0.65) H12A(0.35) C13B(0.35) C14B(0.65) H14B(0.65) N1(0.65) N1A(0.35)
 N2(0.35) N2A(0.65) O9(0.65) C18(0.5) H18(0.5) C19(0.5) C20(0.5) H20(0.5)
 C21(0.5) H21(0.5) N3(0.5) H3(0.5) C17(0.5) H17(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5)
 C29(0.5) H29(0.5) C28(0.5) H28(0.5) N4(0.5) H4(0.5) C27(0.5) H27(0.5) C26(0.5)
 H26(0.5) O0AA(0.35) C5A(0.35) H5A(0.35) C4A(0.35) C3A(0.35) H3A(0.35)
 C6A(0.65) C2A(0.35) C9A(0.35) C14A(0.35) H14A(0.35) C10A(0.35) H10A(0.35)
 C11A(0.35) C13A(0.65) O1AA(0.5) H1AA(0.5) H1AB(0.5)
8.a Riding coordinates:
 O1AA(H1AA,H1AB)
8.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C22(H22A,H22B), C24(H24A,H24B)
8.c Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C5B(H5B), C7(H7A), C7(H7B), C10B(H10B), C12(H12), C12(H12A),
 C14B(H14B), C18(H18), C20(H20), C21(H21), N3(H3), C17(H17), C29(H29), C28(H28),
  N4(H4), C27(H27), C26(H26), C5A(H5A), C3A(H3A), C14A(H14A), C10A(H10A)
8.d Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,N3,C17), C25(C29,C28,N4,C27,C26)
;
_shelx_res_checksum              37633
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'