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_1546103
_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         'C20 H16 N2 O5 Zn'
_chemical_formula_sum            'C20 H16 N2 O5 Zn'
_chemical_formula_weight         429.72
_chemical_name_common            1
_chemical_name_systematic        Zn(E-ip)(bipy)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                65.925(2)
_cell_angle_beta                 75.649(2)
_cell_angle_gamma                76.069(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0944(3)
_cell_length_b                   10.3898(2)
_cell_length_c                   10.4930(3)
_cell_measurement_reflns_used    15955
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      75.9280
_cell_measurement_theta_min      4.5470
_cell_volume                     961.20(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  '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      111(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2186
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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      -0.1243144000
_diffrn_orient_matrix_UB_12      0.1038512000
_diffrn_orient_matrix_UB_13      -0.0647670000
_diffrn_orient_matrix_UB_21      -0.0942160000
_diffrn_orient_matrix_UB_22      -0.0516339000
_diffrn_orient_matrix_UB_23      0.1451679000
_diffrn_orient_matrix_UB_31      0.0334716000
_diffrn_orient_matrix_UB_32      0.1166057000
_diffrn_orient_matrix_UB_33      0.0367407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23586
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.287
_diffrn_reflns_theta_min         4.579
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94155
_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. 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    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.1109
_exptl_crystal_size_mid          0.0734
_exptl_crystal_size_min          0.0619
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0263P)^2^+0.5828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3751
_reflns_number_total             3974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01195d2.cif
_cod_data_source_block           as362_red
_cod_database_code               1546103
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn N O C H'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5B-C9B = O5A-C9A
 1.43 with sigma of 0.01
 C8A-C2 = C8B-C2 = C8A-C7A = C8B-C7B = C7A-C6A = C6B-C7B = C6A-C4 = C6B-C4
 1.4 with sigma of 0.01
 C10B-C9B = C10A-C9A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9B) \\sim Ueq, Uanis(C10B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5B) = Uanis(O5A)
Uanis(C8A) = Uanis(C8B)
Uanis(C7A) = Uanis(C7B)
Uanis(C6A) = Uanis(C6B)
4. Others
 Sof(O5B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C7B)=Sof(C8B)=Sof(H8B)=Sof(C6B)=
 Sof(H6B)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(O5A)=Sof(C8A)=Sof(H8A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C9B(H9BA,H9BB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C17(H17), C3(H3), C14(H14), C20(H20), C8A(H8A), C6A(H6A),
 C8B(H8B), C6B(H6B)
5.c Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F)
;
_olex2_submission_special_instructions 'No special instructions were received'