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_7229195
_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         '0.13(C296 H176 N32 O64 Zn16)'
_chemical_formula_sum            'C49 H50 N8 O12 Zn2'
_chemical_formula_weight         1073.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-17 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            8
_cell_length_a                   21.7570(4)
_cell_length_b                   21.7570(4)
_cell_length_c                   34.6535(11)
_cell_measurement_reflns_used    17577
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      71.9550
_cell_measurement_theta_min      4.0410
_cell_volume                     16403.8(7)
_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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.750
_diffrn_measured_fraction_theta_max 0.740
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.750
_diffrn_reflns_Laue_measured_fraction_max 0.740
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56809
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.056
_diffrn_reflns_theta_min         3.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85320
_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            colorless
_exptl_crystal_density_diffrn    0.870
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.704
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3216
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.716
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.1169
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3989
_refine_ls_wR_factor_ref         0.4342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1998
_reflns_number_total             3216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           Cpd-2a-s16prr168_sq
_cod_original_cell_volume        16403.8(8)
_cod_database_code               7229195
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'colorless tablet'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N2-C12 = C12-C13 = N2A-C12
 1.42 with sigma of 0.005
 C5A-C4A = C5-C4
 1.4 with sigma of 0.005
 C6A-C5A = C5-C6
 1.4 with sigma of 0.005
 C6_$4-C6_$5 \\sim C6A_$4-C6A_$5 \\sim C5_$5-C4_$5 \\sim C5_$5-C6_$5 \\sim
C5A_$5-C4A_$5 ~
 C5A_$5-C6A_$5 \\sim C2-C4 \\sim C2-C4A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N1 \\sim C7 \\sim C8 \\sim C7 \\sim C9 \\sim C10 \\sim C11: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.005
C3 \\sim C4 \\sim C3A \\sim C4A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: N2(0.25) H2(0.125) N2A(0.25) H2A(0.125) N1(0.5) C11(0.5) H11(0.5)
 C10(0.5) H10(0.5) C9(0.5) C8(0.5) H8(0.5) C7(0.5) H7(0.5) C13(0.25) H13(0.25)
 C3(0.5) H3(0.5) C4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C3A(0.5) H3A(0.5)
 C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C12(0.5)
 Fixed Uiso: C5(0.2) C6(0.3) C5A(0.2) C6A(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N2A(H2A), C11(H11), C10(H10), C8(H8), C7(H7), C13(H13), C3(H3),
 C5(H5), C6(H6), C3A(H3A), C5A(H5A), C6A(H6A)
5.b Fitted hexagon refined as free rotating group:
 N1(C11,C10,C9,C8,C7)
;
_olex2_submission_special_instructions 'No special instructions were received'