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_7229193
_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         '0.25(C148 H88 N16 O32 Zn8)'
_chemical_formula_sum            'C40 H29 N5 O9 Zn2'
_chemical_formula_weight         854.42
_chemical_name_systematic
;
 ?
;
_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             2016-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-17 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.821(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9269(10)
_cell_length_b                   23.8222(11)
_cell_length_c                   8.2020(2)
_cell_measurement_reflns_used    13116
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.3790
_cell_measurement_theta_min      3.8620
_cell_volume                     4254.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            74335
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.185
_refine_diff_density_max         1.778
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0713P)^2^+11.4366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6731
_reflns_number_total             9743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           cpd-5b-e16prr56_sq
_cod_database_code               7229193
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Bright yellow'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) C31(0.5)
 H31(0.5) C33(0.65) C34(0.65) H34(0.65) C35(0.65) C36(0.65) H36(0.65) C37(0.65)
 H37(0.65) C27A(0.5) C28A(0.5) H28A(0.5) C29A(0.5) C30A(0.5) H30A(0.5)
 C31A(0.5) H31A(0.5) C33A(0.35) C34A(0.35) H34A(0.35) C35A(0.35) H35A(0.35)
 C36A(0.35) C37A(0.35) H37A(0.35)
3.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C4(H4A), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C14(H14),
  C16(H16), C17(H17), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
 C28(H28), C29(H29), C31(H31), C34(H34), C36(H36), C37(H37), C28A(H28A),
 C30A(H30A), C31A(H31A), C34A(H34A), C35A(H35A), C37A(H37A)
;
_shelx_res_checksum              27941
_shelx_fab_checksum              49256