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_7236169
_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         'C68 H48 Co7 N10 O35, 2(H2 O), 2(H2 O)'
_chemical_formula_sum            'C68 H56 Co7 N10 O39'
_chemical_formula_weight         2049.73
_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             2016-07-06
_audit_creation_method
;
Olex2 1.2-beta
(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                98.732(2)
_cell_angle_beta                 107.645(2)
_cell_angle_gamma                109.102(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5995(2)
_cell_length_b                   12.1967(3)
_cell_length_c                   16.3411(4)
_cell_measurement_reflns_used    13841
_cell_measurement_temperature    288.53(10)
_cell_measurement_theta_max      71.4310
_cell_measurement_theta_min      4.5380
_cell_volume                     1826.92(9)
_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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      288.53(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   57.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  -30.0000 50

  2 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -180.0000 84

  3 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000 -150.0000 73

  4 omega  -32.00   62.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000  -30.0000 94

  5 omega  -32.00   62.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -77.0000   90.0000 94

  6 omega  -34.00   54.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -38.0000   60.0000 88

  7 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   30.0000 95

  8 omega   16.00  104.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000  -60.0000 88

  9 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  -30.0000 73

 10 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000   30.0000 84

 11 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000   90.0000 95

 12 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -150.0000 84

 13 omega  -32.00   52.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -57.0000  -30.0000 84

 14 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91

 15 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 16 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

 17 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 18 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -90.0000 71

 19 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

 20 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

 21 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

 22 omega   40.00  135.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 95

 23 omega   38.00  116.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000   60.0000 78

 24 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -60.0000 71

 25 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 26 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

 27 omega   40.00   98.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

 28 omega   38.00   91.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

 29 omega   40.00   98.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

 30 omega   39.00  110.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

 31 omega   40.00  135.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 95

 32 omega   57.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  178.0000  120.0000 50

 33 omega  -36.00   65.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -19.0000  150.0000 101

 34 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  -90.0000 95

 35 omega   16.00  104.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   38.0000 -150.0000 88

 36 omega  -32.00   52.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -57.0000 -120.0000 84

 37 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000  150.0000 73

 38 omega    0.00   27.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   93.0000  162.2068 27

 39 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000 -120.0000 84

 40 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000    0.0000 95

 41 omega   18.00  102.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   57.0000  -30.0000 84

 42 omega    1.00   74.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203  -99.0000   60.0000 73

 43 omega    6.00  107.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   19.0000 -180.0000 101

 44 omega    8.00  103.00   1.0000    2.1450
omega____ theta____ kappa____ phi______ frames
    -       35.2203   77.0000  -30.0000 95

 45 omega   87.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -90.0000 91

 46 omega   70.00  178.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000    0.0000 108

 47 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

 48 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 49 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

 50 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 51 omega   81.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 52 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 85

 53 omega   87.00  166.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  120.0000 79

 54 omega   91.00  176.00   1.0000   12.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85
;
_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      -0.1258670000
_diffrn_orient_matrix_UB_12      -0.0945098000
_diffrn_orient_matrix_UB_13      0.0122188000
_diffrn_orient_matrix_UB_21      -0.0951822000
_diffrn_orient_matrix_UB_22      -0.0252777000
_diffrn_orient_matrix_UB_23      -0.0987034000
_diffrn_orient_matrix_UB_31      0.0519017000
_diffrn_orient_matrix_UB_32      -0.0990048000
_diffrn_orient_matrix_UB_33      -0.0268333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.648
_diffrn_reflns_theta_min         4.563
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26893
_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 pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1031
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7067
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5876
_reflns_number_total             7067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1826.91(8)
_cod_database_code               7236169
_chemical_oxdiff_formula         'C1 H1 N1 O1 Co1'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(O9)=1-FVAR(1)
 Sof(O10)=FVAR(1)
 Sof(O5W)=1-FVAR(2)
 Sof(O5WA)=FVAR(2)
 Fixed Sof: O15(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O16(H16), O4W(H4WA,H4WB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C19(H19), C21(H21),
 C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
  C34(H34)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'