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_7236170
_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         '0.13(C416 H336 N64 Ni40 O208), 4(H2 O)'
_chemical_formula_sum            'C52 H50 N8 Ni5 O30'
_chemical_formula_weight         1560.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_audit_update_record
;
2016-08-25 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.84540(14)
_cell_length_b                   28.3935(3)
_cell_length_c                   34.5364(3)
_cell_measurement_reflns_used    24770
_cell_measurement_temperature    291.57(10)
_cell_measurement_theta_max      71.3890
_cell_measurement_theta_min      5.5680
_cell_volume                     11615.7(2)
_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      291.57(10)
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   57.00  109.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000 -150.0000 52

  2 omega  -32.00   56.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -38.0000   30.0000 88

  3 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000 -150.0000 84

  4 omega   57.00  109.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000  -30.0000 52

  5 omega  -31.00   64.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -77.0000    0.0000 95

  6 omega   39.00  110.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 71

  7 omega   41.00  126.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 85

  8 omega   40.00   98.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 58

  9 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 10 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 11 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -28.0000 -134.0000 53

 12 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 13 omega   38.00   91.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 14 omega   40.00   98.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 15 omega   41.00  126.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -30.0000 85

 16 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000   30.0000 84

 17 omega   10.00  105.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000  120.0000 95

 18 omega   20.00  104.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000   90.0000 84

 19 omega   18.00  106.00   1.0000    2.5300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   38.0000    0.0000 88

 20 omega   70.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 108

 21 omega   87.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 91

 22 omega   70.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

 23 omega   38.00  116.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000    0.0000 78

 24 omega   90.00  175.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 85

 25 omega   91.00  148.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   90.0000 57

 26 omega   87.00  178.00   1.0000   13.1300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91
;
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            51611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.570
_diffrn_reflns_theta_min         4.242
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45996
_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 greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             6384
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5660
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0622P)^2^+52.4618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5357
_reflns_number_total             5660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01287f2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               7236170
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H13 of C13, H26 of C26, H25 of C25, H18 of C18, H21 of
  C21, H23 of C23, H17 of C17, H15 of C15, H24 of C24, H20 of C20, H3A of C3A,
  H3B of C3B, H5A of C5A, H5B of C5B, H11 of C11
 At 1.5 times of:
  All O(H) groups, H6 of C26, All O(H,H) groups
2. Restrained distances
 C7-C2B \\sim C7-C2A \\sim C3A-C2A \\sim C3B-C2B
 with sigma of 0.02
 N0-C4A \\sim N0A-C4B
 with sigma of 0.02
3. Rigid bond restraints
 O5, N0, C4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O5 \\sim N0 \\sim C4A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C6A) \\sim Ueq, Uanis(C6B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C2B) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5WA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O5, N0, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N0A, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Others
 Fixed Sof: O5(0.5) O11(0.5) N0(0.5) N0A(0.5) C2A(0.5) C2B(0.5) C3A(0.5)
 H3A(0.5) C3B(0.5) H3B(0.5) C4A(0.5) C4B(0.5) C5A(0.5) H5A(0.5) C5B(0.5)
 H5B(0.5) C6A(0.5) C6B(0.5) H7B(0.5) H7A(0.5) O5WA(0.2) H5WA(0.2) H5WB(0.2)
 O5WB(0.8) H5WC(0.8) H5WD(0.8) O6W(0.8) H6WA(0.8) H6WB(0.8) O7W(0.2) H7WA(0.2)
 H7WB(0.2)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2W), O3W(H3WA,H3WB), O4W(H4W), O5WA(H5WA,H5WB),
 O5WB(H5WC,H5WD), O6W(H6WA,H6WB), O7W(H7WA,H7WB)
7.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C7(H7B), C7(H7A), C11(H11), C13(H13),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26)
;
_shelx_res_checksum              31117
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'