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_7229199
_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         '2(C42 H28 N8 O8 Zn2), 4(C3 H7 N O)'
_chemical_formula_sum            'C96 H84 N20 O20 Zn4'
_chemical_formula_weight         2099.31
_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                   16.5520(2)
_cell_length_b                   18.8640(2)
_cell_length_c                   29.4330(3)
_cell_measurement_reflns_used    129821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     9190.07(17)
_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 0.994
_diffrn_measured_fraction_theta_max 0.995
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            125929
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.589
_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    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.275
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.488(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         20994
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0250P)^2^+5.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                16236
_reflns_number_total             20994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           Cpd-1-h09adb09
_cod_database_code               7229199
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.512(9) 0.488(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C89-O19 \\sim C89A-O19A \\sim C86-O20
 with sigma of 0.02
 C89-N19 \\sim C89A-N19 \\sim C86-N20
 with sigma of 0.02
 N19-C90 \\sim N19-C91 \\sim N19-C90A \\sim N19-C91A \\sim N20-C87
 with sigma of 0.02
 O19-C90 \\sim O20-C87
 with sigma of 0.02
4. Others
 Fixed Sof: O19(0.65) O19A(0.35) C89(0.65) H89(0.65) C90(0.65) H90A(0.65)
 H90B(0.65) H90C(0.65) C91(0.65) H91A(0.65) H91B(0.65) H91C(0.65) C89A(0.35)
 H89A(0.35) C90A(0.35) H90D(0.35) H90E(0.35) H90F(0.35) C91A(0.35) H91D(0.35)
 H91E(0.35) H91F(0.35)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N11(H11A), N14(H14), C1(H1), C2(H2), C4(H4), C5(H5), C7(H7),
 C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C19(H19), C20(H20),
  C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C31(H31), C32(H32),
 C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44),
  C46(H46), C47(H47), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55),
 C59(H59), C60(H60), C62(H62), C63(H63), C67(H67), C68(H68), C70(H70), C71(H71),
  C73(H73), C74(H74), C76(H76), C77(H77), C79(H79), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C89(H89), C92(H92), C95(H95), C89A(H89A)
5.b Idealised Me refined as rotating group:
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,
 H91C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C97(H97A,
 H97B,H97C), C90A(H90D,H90E,H90F), C91A(H91D,H91E,H91F)
;
_olex2_submission_special_instructions 'No special instructions were received'