Linker functionalisation triggers an alternative 3D-topology for Zn-isophthalate-4,4′-bipyridine frameworks
Schneemann, Andreas; Rudolf, Robin; Henke, Sebastian; Takahashi, Yukiko; Banh, Hung; Hante, Inke; Schneider, Christian; Noro, Shin-ichiro; Fischer, Roland A.; Dalton Transactions 46 (2017) 8198–8203; doi:10.1039/C7DT01195D

data_1546101
_publ_section_title
;
 Linker functionalisation triggers an alternative 3D-topology for
 Zn-isophthalate-4,4&#x2032;-bipyridine frameworks
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              8198
_journal_page_last               8203
_journal_paper_doi               10.1039/C7DT01195D
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '0.25(C84 H72 N8 O20 Zn4)'
_chemical_formula_sum            'C21 H18 N2 O5 Zn'
_chemical_formula_weight         442.73
_chemical_name_common            2
_chemical_name_systematic        Zn(P-ip)(bipy)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4960(7)
_cell_length_b                   15.8918(6)
_cell_length_c                   11.4039(4)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    240.00(14)
_cell_measurement_theta_max      74.5690
_cell_measurement_theta_min      3.8330
_cell_volume                     2989.5(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -81.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8552  -57.0000   90.0000 63

  2 omega  -97.00  -64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8552  125.0000  -60.0000 33

  3 omega  -34.00   67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8552  -38.0000  -60.0000 101

  4 omega   63.00  109.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  120.0000 46

  5 omega   35.00   60.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 25

  6 omega   38.00  104.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -150.0000 66

  7 omega   46.00   76.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 30

  8 omega   40.00   65.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 25

  9 omega   77.00  139.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 62

 10 omega   69.00  150.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  -60.0000 81

 11 omega -124.00  -99.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -99.0000   90.0000 25

 12 omega   58.00  113.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.4802  175.0000  -60.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0817840000
_diffrn_orient_matrix_UB_12      -0.0409798000
_diffrn_orient_matrix_UB_13      -0.0316762000
_diffrn_orient_matrix_UB_21      0.0418498000
_diffrn_orient_matrix_UB_22      0.0863565000
_diffrn_orient_matrix_UB_23      0.0099541000
_diffrn_orient_matrix_UB_31      0.0166195000
_diffrn_orient_matrix_UB_32      -0.0164316000
_diffrn_orient_matrix_UB_33      0.1309224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9046
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.264
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65638
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_recrystallization_method 'Solvothermal Synthesis'
_exptl_crystal_size_max          0.2617
_exptl_crystal_size_mid          0.1137
_exptl_crystal_size_min          0.0781
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+1.8245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2741
_reflns_number_total             3240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01195d2.cif
_cod_data_source_block           as358b_red_till_run_12
_cod_database_code               1546101
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn O5 N2 C21 H18'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O5B-C9B = O5A-C9A
 1.43 with sigma of 0.01
 C10A-C9A
 1.54 with sigma of 0.01
 C10A-C11A
 1.54 with sigma of 0.01
 C10B-C9B
 1.54 with sigma of 0.01
 C11B-C10B
 1.54 with sigma of 0.01
 C10B-C11C
 1.54 with sigma of 0.01
 C11A-C9A
 2.52 with sigma of 0.02
 C9B-C11B
 2.52 with sigma of 0.02
 C11C-C9B
 2.52 with sigma of 0.02
 O5A-C7A \\sim O5B-C7B
 with sigma of 0.02
 O5A-C9A \\sim O5B-C9B
 with sigma of 0.02
 C2-C8A \\sim C8B-C2 \\sim C6B-C4 \\sim C4-C6A
 with sigma of 0.02
 C7B-C8B \\sim C7A-C8A \\sim C7B-C6B \\sim C7A-C6A
 with sigma of 0.02
 N1-C12B \\sim N1-C12A \\sim N1-C16B \\sim N1-C16A
 with sigma of 0.02
 C16B-C15B \\sim C15A-C16A \\sim C13B-C12B \\sim C13A-C12A
 with sigma of 0.02
 C15A-C14 \\sim C15B-C14 \\sim C13A-C14 \\sim C13B-C14
 with sigma of 0.02
 C10A-C9A \\sim C10B-C9B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12B) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13B) \\sim Ueq,
Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C15B) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8B) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C6A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7A) \\sim Ueq, Uanis(C7B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5B) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(C9B)=Sof(C10B)=Sof(C8B)=Sof(H8B)=0.5*
 (1-FVAR(2))
 Sof(C11B)=Sof(C11C)=0.25*(1-FVAR(2))
 Sof(C6A)=Sof(H6A)=Sof(O5A)=Sof(C7A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C8A)=
 Sof(H8A)=0.5*FVAR(2)
 Fixed Sof: C12A(0.5) H12A(0.5) C16A(0.5) H16A(0.5) C15A(0.5) H15A(0.5)
 C13A(0.5) H13A(0.5) C15B(0.5) H15B(0.5) C13B(0.5) H13B(0.5) C16B(0.5)
 H16B(0.5) C12B(0.5) H12B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C12A(H12A), C16A(H16A), C15A(H15A), C13A(H13A), C15B(H15B),
 C13B(H13B), C16B(H16B), C12B(H12B), C6A(H6A), C6B(H6B), C8A(H8A), C8B(H8B)
;
_olex2_submission_special_instructions 'No special instructions were received'