The impact of N,N′-ditopic ligand length and geometry on the structures of zinc-based mixed-linker metal‒organic frameworks
Burrows, Andrew D.; Chan, Siobhan; Gee, William J.; Mahon, Mary F.; Richardson, Christopher; Sebestyen, Viorica M.; Turski, Domenyk; Warren, Mark R.; CrystEngComm  (2017) –; doi:10.1039/C7CE01447C

data_7229198
_publ_section_title
;
 The impact of N,N&#x2032;-ditopic ligand length and geometry on the
 structures of zinc-based mixed-linker metal--organic frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01447C
_journal_year                    2017
_chemical_formula_moiety         '2(C50 H32 N8 O8 Zn2)'
_chemical_formula_sum            'C112 H92 N20 O20 Zn4'
_chemical_formula_weight         2299.53
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-09 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                116.099(8)
_cell_angle_beta                 112.218(10)
_cell_angle_gamma                97.506(7)
_cell_formula_units_Z            2
_cell_length_a                   18.532(2)
_cell_length_b                   20.3541(15)
_cell_length_c                   20.561(2)
_cell_measurement_reflns_used    3135
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1529
_cell_measurement_theta_min      2.7165
_cell_volume                     6022.3(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.602
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_av_unetI/netI     0.2863
_diffrn_reflns_Laue_measured_fraction_full 0.602
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24223
_diffrn_reflns_point_group_measured_fraction_full 0.602
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.966
_diffrn_reflns_theta_min         2.996
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.950
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         13116
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.2341
_refine_ls_R_factor_gt           0.1463
_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^)+(0.1699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3576
_refine_ls_wR_factor_ref         0.4158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4496
_reflns_number_total             13116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           Cpd-2b-p11mfm2
_cod_original_cell_volume        6022.4(11)
_cod_database_code               7229198
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5A-C12A = C34-C41
 1.54 with sigma of 0.005
 C6A-C11A = C31-C40 = C6A-C10A = C5-C6
 1.4 with sigma of 5
 O1-O2 = O3-O4 = O5-O6 = O7-O8
 2.22 with sigma of 0.005
 O1A-O2A = O3A-O4A = O5A-O6A = O7A-O8A
 2.22 with sigma of 0.005
 C1-O1 = C1-O2
 1.28 with sigma of 0.005
 C12-O3 = C12-O4
 1.28 with sigma of 0.005
 C30-O5 = C30-O6
 1.28 with sigma of 0.005
 C41-O7 = C41-O8
 1.28 with sigma of 0.005
 C1A-O1A = C1A-O2A
 1.28 with sigma of 0.005
 C12A-O3A = C12A-O4A
 1.28 with sigma of 0.005
 C30A-O5A = C30A-O6A
 1.28 with sigma of 0.005
 C41A-O7A = C41A-O8A
 1.28 with sigma of 0.005
 C12A-C4A \\sim C12A-C6A
 with sigma of 0.02
 O4A-C4A \\sim O3A-C6A
 with sigma of 0.02
 C41-C33 \\sim C41-C35
 with sigma of 0.02
 O7-C41 \\sim O8-C41
 with sigma of 0.02
 O7-C33 \\sim O8-C35
 with sigma of 0.02
 C2A-C8A \\sim C5A-C11A
 with sigma of 0.005
 C5A-C4A \\sim C6A-C5A \\sim C7A-C6A \\sim C7A-C2A \\sim C3A-C2A \\sim C4A-C3A
 with sigma of 0.005
 C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C7A-C6A \\sim C7A-C2A
 with sigma of 0.005
 C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C7A
 with sigma of 0.02
 C1-C3 \\sim C1-C11
 with sigma of 0.005
 C3-C2 \\sim C2-C11
 with sigma of 0.005
 C2-C11 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C6-C11
 with sigma of 0.005
 O5A-C31A \\sim O6A-C31A
 with sigma of 0.005
3. Restrained planarity
 C31, C32, C33, C34, C41
 with sigma of 0.1
 O3A, C4A, C5A, C12A, O4A
 with sigma of 0.1
 C2A, C3A, C4A, C5A, C6A, C7A, C12A
 with sigma of 0.1
 O1, O2, C1, C2, C3, C11
 with sigma of 0.1
 O4A, C12A, O3A, C5A
 with sigma of 0.1
4. Others
 Fixed Uiso: O7(0.12) O3A(0.12) C8A(0.1) C11A(0.1) C10A(0.1) C9A(0.1) O4A(0.12)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18), N2(H2), C25(H25), C26(H26), C28(H28),
 C29(H29), C43(H43), C44(H44), C46(H46), C47(H47), N6(H6), C54(H54), C55(H55),
 C57(H57), C58(H58), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20),
  C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C49(H49),
 C14A(H14A), C15A(H15A), C17A(H17A), C18A(H18A), N3A(H3A), C25A(H25A),
 C26A(H26A), C28A(H28A), C29A(H29A), C43A(H43A), C44A(H44A), C46A(H46A),
 C47A(H47A), N7A(H7A), C54A(H54A), C55A(H55A), C57A(H57A), C58A(H58A),
 C3A(H3AA), C4A(H4A), C8A(H8A), C11A(H11A), C10A(H10A), C9A(H9A), C20A(H20A),
 C32A(H32A), C33A(H33A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A),
 C52A(H52A)
5.b Fitted hexagon refined as free rotating group:
 N1(C14,C15,C16,C17,C18), N4(C25,C26,C27,C28,C29), N5(C43,C44,C45,C46,C47),
 N8(C54,C55,C56,C57,C58), C6(C7,C8,C9,C10,C11), C31(C32,C33,C34,C35,C40),
 N1A(C14A,C15A,C16A,C17A,C18A), N4A(C25A,C26A,C27A,C28A,C29A), N5A(C43A,C44A,
 C45A,C46A,C47A), N8A(C54A,C55A,C56A,C57A,C58A), C8A(C7A,C6A,C11A,C10A,C9A),
 C31A(C32A,C33A,C34A,C35A,C36A)
;
_olex2_submission_special_instructions 'No special instructions were received'