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_7236173
_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 Cd3 N4 O18, 2(C2 H8 N), 3(H2 O)'
_chemical_formula_sum            'C36 H34 Cd3 N6 O21'
_chemical_formula_weight         1223.89
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                111.3156(19)
_cell_angle_beta                 102.5684(18)
_cell_angle_gamma                93.8625(17)
_cell_formula_units_Z            1
_cell_length_a                   9.8669(2)
_cell_length_b                   10.4250(2)
_cell_length_c                   12.4397(3)
_cell_measurement_reflns_used    13779
_cell_measurement_temperature    290.56(17)
_cell_measurement_theta_max      71.4660
_cell_measurement_theta_min      4.6150
_cell_volume                     1148.29(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.56(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  -30.0000 101

  2 omega    1.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000   90.0000 75

  3 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -180.0000 94

  4 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  150.0000 84

  5 omega    2.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   91.0000  -75.3243 27

  6 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000 -180.0000 94

  7 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   30.0000 84

  8 omega   13.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -113.0000  -13.0000 70

  9 omega   40.00   98.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

 10 omega   38.00   91.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 11 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 71

 12 omega   38.00   91.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

 13 omega   38.00  116.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000  -30.0000 78

 14 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

 15 omega   57.00  150.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 93

 16 omega   37.00  146.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000  120.0000 109

 17 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

 18 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -30.0000 85

 19 omega   39.00  110.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 71

 20 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 21 omega   41.00  126.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  120.0000 85

 22 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000    0.0000 84

 23 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   90.0000 84

 24 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -30.0000 84

 25 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -150.0000 94

 26 omega   57.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000 -150.0000 52

 27 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000 -120.0000 84

 28 omega   70.00  178.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

 29 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

 30 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

 31 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

 32 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

 33 omega   70.00  178.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 108

 34 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 35 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 95

 36 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -90.0000 85

 37 omega   90.00  175.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  120.0000 85

 38 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 39 omega   91.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 85

 40 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  150.0000 101

 41 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -60.0000 84

 42 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   30.0000 94

 43 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000    0.0000 84

 44 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   38.0000  -60.0000 88

 45 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  120.0000 94

 46 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

 47 omega   81.00  176.00   1.0000    1.4300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0376607000
_diffrn_orient_matrix_UB_12      0.0316538000
_diffrn_orient_matrix_UB_13      -0.1136650000
_diffrn_orient_matrix_UB_21      -0.0711363000
_diffrn_orient_matrix_UB_22      -0.1526990000
_diffrn_orient_matrix_UB_23      -0.0731865000
_diffrn_orient_matrix_UB_31      -0.1406856000
_diffrn_orient_matrix_UB_32      0.0389102000
_diffrn_orient_matrix_UB_33      0.0261166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21241
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.546
_diffrn_reflns_theta_min         4.613
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0628P)^2^+2.5296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4250
_reflns_number_total             4417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           5
_cod_original_cell_volume        1148.29(4)
_cod_database_code               7236173
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cd1'
_reflns_odcompleteness_completeness 99.95
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N3-C17 = N3-C18
 1.4 with sigma of 0.01
 C18-C17
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C17, C18, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O10)=1-FVAR(1)
 Sof(O9)=FVAR(1)
 Fixed Sof: O2W(0.5) H2Wa(0.5) H2Wb(0.5)
6.a Riding coordinates:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), O1W(H1Wa,H1Wb), O2W(H2Wa,H2Wb)
6.b Secondary CH2 refined with riding coordinates:
 N3(H3a,H3b)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'