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_7236174
_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 Co3 N4 O18, H2 O, C13 H16 N2'
_chemical_formula_sum            'C45 H30 Co3 N6 O19'
_chemical_formula_weight         1135.54
_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             2016-08-18
_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                112.322(2)
_cell_angle_beta                 101.936(2)
_cell_angle_gamma                92.9815(19)
_cell_formula_units_Z            1
_cell_length_a                   9.6701(2)
_cell_length_b                   10.2782(2)
_cell_length_c                   11.9406(3)
_cell_measurement_reflns_used    7018
_cell_measurement_temperature    288.85(12)
_cell_measurement_theta_max      71.1530
_cell_measurement_theta_min      4.6890
_cell_volume                     1062.89(5)
_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_environment      air
_diffrn_ambient_temperature      288.85(12)
_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 0.989
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000   60.0000 94

  2 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -90.0000 84

  3 omega  -35.00   66.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000 -180.0000 101

  4 omega   57.00  109.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000   90.0000 52

  5 omega  -35.00   66.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000  -90.0000 101

  6 omega    1.00   76.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000 -150.0000 75

  7 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -180.0000 84

  8 omega    1.00   76.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000  -30.0000 75

  9 omega   40.00   98.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 10 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

 11 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

 12 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 85

 13 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 71

 14 omega   41.00  126.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 85

 15 omega   38.00  116.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -150.0000 78

 16 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 17 omega   39.00  110.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -30.0000 71

 18 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 19 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 20 omega   38.00   91.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 21 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

 22 omega   40.00   98.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

 23 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

 24 omega   70.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  120.0000 108

 25 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   60.0000 94

 26 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   90.0000 84

 27 omega   20.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000    0.0000 84

 28 omega  -31.00   53.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000  120.0000 84

 29 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   90.0000 94

 30 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  -60.0000 94

 31 omega   10.00  104.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -150.0000 94

 32 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

 33 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 95

 34 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 35 omega   91.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

 36 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 37 omega   87.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 91

 38 omega   81.00  176.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 39 omega   70.00  178.00   1.0000    5.4800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108
;
_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      0.1568920000
_diffrn_orient_matrix_UB_12      -0.0096806000
_diffrn_orient_matrix_UB_13      -0.0061544000
_diffrn_orient_matrix_UB_21      0.0028298000
_diffrn_orient_matrix_UB_22      0.1278828000
_diffrn_orient_matrix_UB_23      -0.0373239000
_diffrn_orient_matrix_UB_31      0.0495481000
_diffrn_orient_matrix_UB_32      0.1018002000
_diffrn_orient_matrix_UB_33      0.1388026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.504
_diffrn_reflns_theta_min         4.128
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43387
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             575
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4104
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0508P)^2^+1.1550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3675
_reflns_number_total             4104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           6
_cod_original_cell_volume        1062.88(5)
_cod_database_code               7236174
_chemical_oxdiff_formula         'C1 H1 N1 O1 Co1'
_reflns_odcompleteness_completeness 99.97
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C5A, C6, C6A, C7, C7A, C8, C9, C10, C11, C12, C13, C14,
 C15, C16, C18, C19, C20, C21, C17, C22, C23, C24, C25, C29, C28, C27, C26, N1,
 N1A, N2, N2A, N4, N3, O5, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O5)=Sof(N1)=Sof(N2)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(O5A)=Sof(N1A)=Sof(N2A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=FVAR(1)
 Fixed Sof: O1W(0.5) H1Wa(0.5) H1Wb(0.5) C18(0.5) H18(0.5) C19(0.5) C20(0.5)
 H20(0.5) C21(0.5) H21(0.5) N4(0.5) H4(0.5) C17(0.5) H17(0.5) C22(0.5)
 H22a(0.5) H22b(0.5) C23(0.5) H23a(0.5) H23b(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) N3(0.5) H3a(0.5) C27(0.5)
 H27(0.5) C26(0.5) H26(0.5)
5.a Riding coordinates:
 O1W(H1Wa,H1Wb)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C5A(H5A), C7(H7), C7A(H7A), C10(H10), C12(H12), C14(H14),
 C18(H18), C20(H20), C21(H21), N4(H4), C17(H17), C29(H29), C28(H28), N3(H3a),
 C27(H27), C26(H26)
5.d Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,N4,C17), C25(C29,C28,N3,C27,C26)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'