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_7236175
_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 Mn3 N4 O18, C10 H10 N2, 2(H2 O)'
_chemical_formula_sum            'C42 H26 Mn3 N6 O20'
_chemical_formula_weight         1099.51
_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                112.088(2)
_cell_angle_beta                 101.488(2)
_cell_angle_gamma                94.1132(18)
_cell_formula_units_Z            1
_cell_length_a                   9.7826(2)
_cell_length_b                   10.3101(2)
_cell_length_c                   12.1333(3)
_cell_measurement_reflns_used    11878
_cell_measurement_temperature    289.03(10)
_cell_measurement_theta_max      71.3850
_cell_measurement_theta_min      4.6550
_cell_volume                     1096.65(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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.03(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 0.989
_diffrn_measurement_details
;
  1 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -180.0000 94

  2 omega    7.00  108.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   19.0000  150.0000 101

  3 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  150.0000 84

  4 omega    1.00   76.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000   60.0000 75

  5 omega   55.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203 -178.0000   30.0000 54

  6 omega  -31.00   53.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -57.0000  120.0000 84

  7 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000   30.0000 84

  8 omega  -31.00   63.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -77.0000 -180.0000 94

  9 omega  -32.00   56.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -38.0000 -120.0000 88

 10 omega    1.00   76.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -99.0000 -180.0000 75

 11 omega   38.00  116.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000    0.0000 78

 12 omega   39.00  110.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 71

 13 omega   39.00  110.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -150.0000 71

 14 omega   87.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91

 15 omega   38.00  116.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000  120.0000 78

 16 omega  101.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  112.0000  -60.0000 77

 17 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 85

 18 omega   40.00  135.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   30.0000 95

 19 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

 20 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 21 omega   38.00   91.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

 22 omega   40.00   98.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

 23 omega   37.00  146.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 109

 24 omega   90.00  175.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -120.0000 85

 25 omega   40.00  135.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 95

 26 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   90.0000 94

 27 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000    0.0000 94

 28 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000 -120.0000 94

 29 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  -90.0000 94

 30 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000   60.0000 94

 31 omega   57.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000  -30.0000 52

 32 omega  -35.00   66.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  -19.0000  -30.0000 101

 33 omega   10.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   77.0000  150.0000 94

 34 omega   57.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203  178.0000   90.0000 52

 35 omega   18.00  106.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   38.0000  -90.0000 88

 36 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000 -120.0000 84

 37 omega   20.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -       36.7203   57.0000  -30.0000 84

 38 omega   87.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91

 39 omega   70.00  178.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 108

 40 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 85

 41 omega   90.00  145.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 55

 42 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

 43 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 44 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 85

 45 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 46 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

 47 omega   81.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

 48 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 85

 49 omega   91.00  176.00   1.0000    6.1600
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 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      0.0319963000
_diffrn_orient_matrix_UB_12      0.0197501000
_diffrn_orient_matrix_UB_13      0.1354139000
_diffrn_orient_matrix_UB_21      0.1511231000
_diffrn_orient_matrix_UB_22      0.0735290000
_diffrn_orient_matrix_UB_23      0.0204740000
_diffrn_orient_matrix_UB_31      -0.0515114000
_diffrn_orient_matrix_UB_32      0.1445814000
_diffrn_orient_matrix_UB_33      0.0348693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            20392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.503
_diffrn_reflns_theta_min         4.055
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21553
_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    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             555
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0802P)^2^+0.8834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4007
_reflns_number_total             4219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           7
_cod_original_cell_volume        1096.64(5)
_cod_database_code               7236175
_chemical_oxdiff_formula         'C1 H1 O1 N1 Mn1 Cl1'
_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 N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C21-C20 = C20-C19 = C19-C18 = C18-C17
 1.38 with sigma of 0.01
 C22-C23 = C23-C24 = C22-C26 = C26-C25
 1.38 with sigma of 0.01
 C21-N3 = N3-C17 = C24-N4 = N4-C25
 1.34 with sigma of 0.01
3. Rigid bond restraints
 C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, N3, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O9(0.5) O10(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5)
 C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) N3(0.5) H3a(0.5) N4(0.5) H4(0.5)
 O2W(0.5) H2Wa(0.5) H2Wb(0.5) O1W(0.5) H1Wa(0.5) H1Wb(0.5)
6.a Riding coordinates:
 O2W(H2Wa,H2Wb), O1W(H1Wa,H1Wb)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), N3(H3a), N4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'