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_7229196
_publ_section_title
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 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         'C21 H14 N4 O4 Zn, C3 H7 N O'
_chemical_formula_sum            'C24 H21 N5 O5 Zn'
_chemical_formula_weight         524.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-02
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.14400(10)
_cell_length_b                   13.97600(10)
_cell_length_c                   16.1920(2)
_cell_measurement_reflns_used    65176
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2295.58(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski, Minor 1997)'
_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_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44382
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.534
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;

1 molecule of DMF in the asymmetric unit. C22 and 
C23 disordered over 2 sites in a 60:40 ratio. 
Hydrogen bonding present.
 
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.092(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.9409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4954
_reflns_number_total             5253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           Cpd-3-k10adb14
_cod_database_code               7229196
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.605
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.908(12) 0.092(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: O5(0.6) C22(0.6) H22(0.6) C23(0.6) H23A(0.6) H23B(0.6) H23C(0.6)
 O5A(0.4) C22A(0.4) H22A(0.4) C23A(0.4) H23D(0.4) H23E(0.4) H23F(0.4)
4.a Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C3(H3A), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
  C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C22A(H22A)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'