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_1546100
_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         'C21 H16 N2 O5 Zn'
_chemical_formula_sum            'C21 H16 N2 O5 Zn'
_chemical_formula_weight         441.73
_chemical_name_common            3
_chemical_name_systematic        Zn(A-ip)(bipy)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.451(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3928(3)
_cell_length_b                   15.6359(5)
_cell_length_c                   16.3018(6)
_cell_measurement_reflns_used    5050
_cell_measurement_temperature    102.9(3)
_cell_measurement_theta_max      74.0310
_cell_measurement_theta_min      3.8620
_cell_volume                     2885.56(16)
_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      102.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega -123.00  -79.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000 -150.0000 44

  2 omega -104.00  -45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302 -166.0000   15.0000 59

  3 omega -109.00  -52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000   60.0000 57

  4 omega   50.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  166.0000   37.0000 73

  5 omega   48.00   77.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000   60.0000 29

  6 omega   34.00   59.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  150.0000 25

  7 omega   31.00   69.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  -90.0000 38

  8 omega   37.00   66.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -150.0000 29

  9 omega   45.00   77.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000 -120.0000 32

 10 omega   87.00  151.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000   30.0000 64

 11 omega   35.00   62.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  -60.0000 27

 12 omega   32.00   66.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000   90.0000 34

 13 omega   98.00  125.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  125.0000  -90.0000 27

 14 omega  132.00  158.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  125.0000  -90.0000 26

 15 omega   46.00   76.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000 -180.0000 30

 16 omega   86.00  156.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000   90.0000 70

 17 omega   32.00   59.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  120.0000 27
;
_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      0.0209295000
_diffrn_orient_matrix_UB_12      -0.0369917000
_diffrn_orient_matrix_UB_13      -0.0846903000
_diffrn_orient_matrix_UB_21      -0.1085637000
_diffrn_orient_matrix_UB_22      0.0490375000
_diffrn_orient_matrix_UB_23      -0.0405569000
_diffrn_orient_matrix_UB_31      0.0792978000
_diffrn_orient_matrix_UB_32      0.0770937000
_diffrn_orient_matrix_UB_33      -0.0148964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.111
_diffrn_reflns_theta_min         3.905
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62704
_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    1.017
_exptl_crystal_description       plank
_exptl_crystal_F_000             904
_exptl_crystal_recrystallization_method 'Solvothermal Synthesis'
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.0611
_exptl_crystal_size_min          0.0437
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5691
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0944P)^2^+3.0083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5121
_reflns_number_total             5691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01195d2.cif
_cod_data_source_block           ascid-allyloxy_red
_cod_database_code               1546100
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C21 H17 N2 O5'
_reflns_odcompleteness_completeness 99.93
_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
2. Restrained distances
 C11A-C10 \\sim C11B-C10
 with sigma of 0.02
 C18B-C17 \\sim C17-C18A \\sim C21A-C17 \\sim C21B-C17
 with sigma of 0.02
 N2-C19A \\sim N2-C19B \\sim N2-C20B \\sim N2-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21A) \\sim Ueq, Uanis(C21B) \\sim Ueq, Uanis(C20B) \\sim Ueq,
Uanis(C20A) \\sim Ueq, Uanis(C19B) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C19B(0.5) H19B(0.5) C19A(0.5) H19A(0.5) C18A(0.5) H18A(0.5)
 C21B(0.5) H21B(0.5) C20B(0.5) H20B(0.5) C20A(0.5) H20A(0.5) C18B(0.5)
 H18B(0.5) C21A(0.5) H21A(0.5) H10A(0.5) H10(0.5) C11A(0.5) H11A(0.5) H11B(0.5)
 C11B(0.5) H11C(0.5) H11D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C8(H8), C15(H15), C13(H13), C19B(H19B), C16(H16), C6(H6),
 C19A(H19A), C18A(H18A), C21B(H21B), C20B(H20B), C20A(H20A), C18B(H18B),
 C21A(H21A), C10(H10A), C10(H10)
5.c X=CH2 refined with riding coordinates:
 C11A(H11A,H11B), C11B(H11C,H11D)
;
_olex2_submission_special_instructions 'No special instructions were received'